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The Vespiary
Main Topics => Drug Synthesis & Extraction => Topic started by: German on December
03, 2009, 08:49:05 PM
Part 1
First you do one of these two LSA extraction methods:
The method is very simple, requires nothing you can't buy easily and legally, and it's
not very expensive. There are refinements galore to this, and I might try them in
order to purify this stuff, but the chemicals aren't as available, and it requires things
like pH paper, which I don't know how to get. Maybe I can get some anyway. I'll see.
First of all, you need either (a) a lot of morning glory seeds or (b) some hawiian baby
woodrose seeds. You also need petroleum ether, which is a petroleum refining
byproduct, and some high proof drinkable ethanol.
I'll explain the theory as I understand it so that you can understand the flexability in
this recipe.
There are two kinds of solvents, polar and nonpolar. Generally, the good stuff in
seeds is polar soluble, and the bad stuff is nonpolar soluble.
So the idea is to first make a nonpolar solution, which of course means that you take
a nonpolar solvent and soak the ground up seeds in it. The result is a solution of
garbage from the seeds and the nonpolar solvent. Petroleum ether is a nonpolar
solvent, so it will function in this capacity. The down side is that petroleum ether is
poisonous, so you don't want to drink it. The good news is that pet. ether is
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extremely volatile, so it evaporates quickly and cleanly. So the first stage is to soak
the ground up seeds in petroleum ether for a few days, and then filter the resulting
cloudy solution through some coffee filters, throw away the solution, and keep the
seed mush. The seed mush consists of nondisolved LSA's, fiber, and the remaining
solution that didn't drip through the filter. This part can be iterated to get more and
more garbage out of the mush. The final time, let the seed mush dry thoroughly so
that the petroleum ether evaporates and you don't have any poison in there.
After the seed mush dries, the nest stage is to make a polar solution, which
separates the alkaloids (the LSA) from the fiber of the seeds. This is done with
alcohol. There are other polar solvents, but again, the key is to have one which easily
evaporates, one which will not destroy the LSA's, and one which is not poisonous.
Ethanol serves this purpose. Methanol will also work, but methanol causes blindness,
so if you use methanol, make damn sure it's all evaporated before consuming the
product. In some states ethanol is illegal, and California is such a state. In that case,
using methanol is probably the way to go. Also keep in mind that there is such thing
as denatured ethanol, which is ethanol which has been intentionally poisoned so that
it is undrinkable. The reason for doing this is that drinkable ethanol is taxable under
the Tobacco Alcohol and Firearms people, and denatured ethanol has uses in
chemistry and cleaning. The point is that you should under no circumstances use
denatured ethanol because it will make you sick or kill you or cause cancer or all
three. So, make an alcohol solution of the seeds. Then filter the solution through
filter paper, like before, except this time keep the liquid in a jar. Repeat this step 3 or
4 times, always keeping the liquid. When you've exhausted the seeds, throw them
away. The liquid you have should be yellow and smelly. Put this in a shallow flat tray
or pan or large bowl, and let it evaporate in a dark dry place for a day or two, or until
there is no liquid. The pan should have a yellowish scum residue. That's the LSA
gunk. Scrape that up with a razor blade or credit card or whatever works. It'll be
sticky and gummy, and once it's all scraped up it will look dark brown.
That's pretty much all there is to it. You can take this several steps further to get a
more pure product. That would be to alternately make an acid solution and base salts
from the LSA's, which would eventually leave you with a very pure white powder.
This requires much more effort, and wastes some of the product, and the only reason
for doing it would be to remove more garbage, but the amount of garbage left in the
brown gunk is insignificant.
Once you have this stuff as pure as you want it, you can ingest it in your favorite
form. You can either swallow it as a lump, put it into a gelatin capsule, drink the
ethanol solution, or dissolve it in some cool-aid. I recommend either capsules or
swallow the lump if you can handle the taste.
Other notes: Petroleum ether is in Naptha, which is available in hardware stores.
That's what I've used, and it works fine. [However, see this warning about Naptha]
Other petroleum solvents would work like ethyl ether, which evaporates much more
easily and is a better solvent, and something like gasoline, which has additives and
does not evaporate as cleanly as naptha. If you can get petroleum ether from a
chemical supplier, try it instead of naptha. A rule of thumb is that after making a
solution with the nonpolar solvent, and after it dries, it should smell absolutely
nothing at all like petroleum, or whatever solvent you used. If you use gasoline,
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you'll notice a strong gasoline smell, which means you're screwed. I know first hand
from repeated experience that naptha works. Also, read the labels of whatever
solvent you use. Make sure it contains no benzene. Benzene is the most evil
carcinogen known, and even in trace amounts it can cause cancer. There is no safe
amount of benzene. On the other hand benzene is everywhere, and if some chemical
engineer points out to you that there is benzene in naptha even if it's not on the label
keep in mind that there is an enormous amount of benzene in automobile exhaust.
You're going to die anyway. If there is no mention of carcinogens or benzene on the
label of the naptha, then there isn't enough such that you should not use it.
The finer details of this recipe I can give you another time, but I just wanted to give
you some theory and a general idea of what the procedure is. I can give you some
things I have from off the net pertaining to this.
-------------------------------------------------------------------------------Subject: Re: Extracting LSA from HBWR
Concerning the extraction and purification of LSA from HBWR, The alkaloids are
more polar than e.g. DMT or mescaline, and are probably water soluble to some
extent. Thus, while a crude extraction can be performed with methanol, the next
stage of purification may not be very good. Thus the general extraction method
for alkaloids is quite possibly not applicable here. That is why I want to have a
look at exactly what the original method was, although the journal seems obscure
to say the least. Another day in the Chem Abs section, I fear.
-------------------------------------------------------------------------------Subject: Re: LSA
>Yup. In a nutshell, you mix the HWBR powder in a nonpolar solvent, keep the
>resultant gunk(I) and throw away the solution. Then dissolve the gunk(I)
>into a polar solvent, throw away the new gunk(II) and evaporate the solution.
>The final gunk (III) that comes out of the solution has LSA in it.
>
> gunk(I) = gunk(II) + gunk(III)
> gunk(III) is the good stuff
> gunk(II) is not
> gunk(I+III) are therefore kept
>
>nonpolar solvent = petroleum ether
>polar solvent = alcohol (methanol is better, but is a smidgin poisinous
> so you've got to be damn sure its all evaporated).
OR
(E.W. Hand) writes :
>Does anyone know about the validity of extracting lysergic acid
>from Hawaiian Wood Rose seeds or Morning Glory seeds. According
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-------------------------------------------------------------------------------EXTRACTION:
The method I use is a general one - I copied it from one used by some scientists to
extract mescaline from peyote, but I have since seen close variations used on many
plants. This procedure is followed, whenever a plant is studied for its alkaloids.
A few ingredients and bits of equipment are necessary. I am a chemist, and have my
own chemistry set. I have considered manufacture, but I find that there are enough
interesting things to do just extracting natural compounds, which is much easier,
indeed, possible in the home.
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Procedure:
Get your stuff.
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Dry it as much as possible - this makes life easier later on. You will never get all the
water out, but too bad.
Chop it up as fine as possible: a blender comes in handy. You may wish to chop then
dry. A word of caution : try to avoid exposing your stuff to excessive heat. I dry in
low heat oven. Heat and air destroy good compounds from upwards of 100 degs C.
All this bit will depend on exactly what you are extracting.
Once it is finely divided - powdered if possible, put it in a big container, and cover it
with methanol. Alternatives to methanol here are ethanol (not as good) and acetone
(good solvent - rips the crap out of anything, but is more reactive - can react with
your actives).
Now, depending on what your stuff is, you have to let the methanol have time to
remove it all. This is best done by leaving in a quiet warm place for a few days, even
up to a week, and shaking it occasionally so it is mixed. Some papers recommend
solvent extraction (soxhlet apparatus) and refluxing at the boiling point of the
methanol (80 degs or so - I can't remember). I usually just rely on time to get the
good stuff out.
When you are ready (early in the morning), filtre the muck, to give you
methanol+dissolved brown gunk, and a residue soaked with methanol. The residue
still contains a lot of good stuff, so soak again for an hour, and repeat, and do a third
time if you are feeling generous (3 is the magic number in extraction work).
When you are done, there is another thing you can do finally, if desired: depending
on what your stuff is, mix it up with dilute hydrochloric acid, 1M is appropriate. let
stand for an hour, then filtre (this may be very difficult) That will get the last of the
alkaloids out of the substrate.
You now have a methanol-plant stuff mixture, and a dilute HCL-plant stuff mixture, if
you bothered to do that part.
Evaporate the methanol, to leave a small amount of goo. This will contain water, a bit
of methanol, and all kinds of resins and muck, and if you are lucky, the alkaloids.
If a very quick and crude extraction was all that was desired, then after stripping the
last of the methanol with vacuum if possible, this residue could be smoked eaten or
whathaveyou. I leave that to your discretion. However, if a cleaner product is
desired, the double layer extraction will need to be performed.
Combine the evaporated methanol gunge with the hydrochloric acid filtrate if you
have any. If you don't then mix the methanol stuff with an excess of dilute (1M) HCl.
Feel free to filtre again at this point. Anything of marginal solubility here is no good
to you. Get the stuff as clean as possible. Boiling with activated charcoal is another
useful trick for removing gunge. Just boil it up, and filter off the charcoal for a cleaner
brew.
You should now have an acid aqueous solution of alkaloids and water solubles from
the plant.
Take your acidic solution, and bassify. This is done by mixing in dilute sodium
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hydroxide (I use up to 5M to save on total volume. Be careful with conc NaOH - apart
from eating skin, it eats alkaloids) As you mix in the NaOH, you will see swirls of
white precipitate form and redissolve. Continue until the white swirls stay, and until
the solution is quite cloudy. Indicator paper is necessary to see that the solution is
basic. If you can't get indicator paper, you can make an indicator by boiling up some
purple flowers. The dyes in most flowers go bright red in acid, and green in strong
alkali. Just a drop of dye and a drop of mixture should tell you what is acid or base.
The white precipitate is the alkaloids. The more the better.
Next, add equal volume of non-polar solvent (dichloromethane) to the mix. Place in
separating funnel, and shake. Separate. This may be very difficult or slow. Adding
more solvent, more basic water, etc. may help. Adding lots of salt to the water layer
will help break an emulsion. Ideally you want it do this step 3 times - to extract as
much as possible from the water layer into the organic. I find this part very difficult,
and you have to accept that you will lose quite a lot of material here. It is, however
probably easier with some plants that others: cactus is very difficult, barks and seeds
would be easier. Use plenty of salt, and agitate to separate. When you have finished
extraction, chuck the basic water layer. The solvent layer is kept, and can be
backwashed with salty water for a cleaner mixture.
The solvent can now be dried, (using salt or some dry powder, the filtred) (I don't
usually bother with this - the old hairdryer at the end can remove some last solvent
and water) then strip the solvent in a vacuum to get your final product - some kind of
syrup could be expected. This is super concentrated, but may only be half the
strength of the original. e.g. put in enough for 10 doses of morning glory seeds, get
back 5 doses or more of concentrated alkaloids.
If it is desired to take the process still further, you can do the obvious thing - mix
your solvent layer with dilute acid again and extract back into water. Acid layer could
be evaporated under vacuum to give salts of alkaloids. Alternatively, if the organic
layer were scrupulously dry, bases could be salted out with some organic acid - a
tartrate, oxalate could be formed. I have never bothered with such things - you
would need a lot of pure extract to be bothered.
The acid-base extraction process can be continued as many times as is desired.
If a truly pure product is desired, the only way to go from here is chromatography. I
have never used this at home, and wouldn't think it was worth the trouble, but there
will be papers available on what was used for a particular extraction case.
Part 2
Then take that LSA and other amides and do this:
LSD-25 Synthesis from "Psychedelic Guide to the Preparation of the Eucharist"
Preparatory arrangements
Starting material may be any lysergic acid derivative, from ergot on rye grain or from
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culture, or morning glory seeds or from synthetic sources. Preparation #1 uses any
amide, or lysergic acid as starting material. Preparations #2 and #3 must start with
lysergic acid only, prepared from the amides as follows:
10 g of any lysergic acid amide from various natural sources dissolved in 200 ml of
methanolic KOH solution and the methanol removed immediately in vacuo. The
residue is treated with 200 ml of an 8% aqueous solution of KOH and the mixture
heated on a steam bath for one hour. A stream of nitrogen gas is passed through the
flask during heating and the evolved NH3 gas may be titrated is HCl to follow the
reaction. The alkaline solution is made neutral to congo red with tartaric acid,
filtered, cleaned by extraction with ether, the aqueous solution filtered and
evaporated. Digest with MeOH to remove some of the coloured material from the
crystals of lysergic acid.
Arrange the lighting in the lab similarly to that of a dark room. Use photographic red
and yellow safety lights, as lysergic acid derivatives are decomposed when light is
present. Rubber gloves must be worn due to the highly poisonous nature of ergot
alkaloids. A hair drier, or, better, a flash evaporator, is necessary to speed up steps
where evaporation is necessary.
Preparation #1
Step I. Use Yellow light
Place one volume of powdered ergot alkaloid material in a tiny roundbottom flask and
add two volumes of anhydrous hydrazine. An alternate procedure uses a sealed tube
in which the reagents are heated at 112 C. The mixture is refluxed (or heated) for 30
minutes. Add 1.5 volumes of H2O and boil 15 minutes. On cooling in the refrigerator,
isolysergic acid hydrazide is crystallised.
Step II. Use Red light
Chill all reagents and have ice handy. Dissolve 2.82 g hydrazine rapidly in 100 ml 0.1
N ice-cold HCl using an ice bath to keep the reaction vessel at 0 C. 100 ml ice-cold
0.1 N NaNO2 is added and after 2 to 3 minutes vigorous stirring, 130 ml more HCl is
added dropwise with vigorous stirring again in an ice bath. After 5 minutes, neutralise
the solution with NaHCO3 saturated sol. and extract with ether. Remove the aqueous
solution and try to dissolve the gummy substance in ether. Adjust the ether solution
by adding 3 g diethylamine per 300 ml ether extract. Allow to stand in the dark,
gradually warming up to 20 C over a period of 24 hours. Evaporate in vacuum and
treat as indicated in the purification section for conversion of iso-lysergic amides to
lysergic acid amides.
Preparation #2
Step I. Use Yellow light
5.36 g of d-lysergic acid are suspended in 125 ml of acetonitrile and the suspension
cooled to about -20 C in a bath of acetone cooled with dry ice. To the suspension is
added a cold (-20 C) solution of 8.82 g of trifluoroacetic anhydride in 75 ml of
acetonitrile. The mixture is allowed to stand at -20 C for about 1.5 hours during
which the suspended material dissolves, and the d-lysergic acid is converted to the
mixed anhydride of lysergic and trifluoroacetic acids. The mixed anhydride can be
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ethylene dichloride. the combined extract is dried and then concentrated to a syrup
under reduced pressure. Do not heat up the syrup during concentration. the LSD may
crystallise out, but the crystals and the mother liquor may be chromatographed
according to the instructions on purification.
Purification of LSD-25
The material obtained by any of these three preparations may contain both lysergic
acid and iso-lysergic acid amides. Preparation #1 contains mostly iso-lysergic
diethylamide and must be converted prior to separation. For this material, go to Step
II first.
Step I
Use darkroom and follow with a long wave UV The material is dissolved in a 3:1
mixture of benzene and chloroform. Pack the chromatography column with a slurry of
basic alumina in benzene so that a 1 inch column is six inches long. Drain the solvent
to the top of the alumina column and carefully add an aliquot of the LSD-solvent
solution containing 50 ml of solvent and 1 g LSD. Run this through the column,
following the fastest moving fluorescent band. After it has been collected, strip the
remaining material from the column by washing with MeOH. Use the UV light
sparingly to prevent excessive damage to the compounds. Evaporate the second
fraction in vacuo and set aside for Step II. The fraction containing the pure LSD is
concentrated in vacuo and the syrup will crystallise slowly. This material may be
converted to the tartrate by tartaric acid and the LSD tartrate conveniently
crystallised. MP 190-196 C.
Step II. Use Red light
Dissolve the residue derived from the methanol stripping of the column in a minimum
amount of alcohol. Add twice that volume of 4 N alcoholic KOH solution and allow the
mixture to stand at room temperature for several hours. Neutralise with dilute HCl,
make slightly basic with NH4OH and extract with chloroform or ethylene dichloride as
in preparations #1 or #2. Evaporate in vacuo and chromatograph as in the previous
step.
Lysergic acid compounds are unstable to heat, light and oxygen. In any form it helps
to add ascorbic acid as an anti- oxidant, keeping the container tightly closed,
light-tight with aluminum foil, and in a refrigerator.
Synthesis of d-LSD maleate or tartrate from lysergic acid with POCl3
Ref:
Johnson, Ary, Teiger, Kassel. "Emetic Activity of Reduced Lysergamides." Journal of
Medicinal Chemistry. 16(5):532-537. 1973.
Related:
Huang, Marona-Lewicka, Pfaff, Nichols. "Drug Discrimination and Receptor Binding
Studies of N-Isopropyl Lysergamide Derivates." Pharmacology, Biochmistry and
Behavior. 47(3):667-673, 1994.
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In order to get anywhere around the amount of LSD worth making (10+grams) you'd
need around 50,000 HBWR. The cheapest I found was 11,000 seeds for 500 dollars.
Assuming you found the right way to extract them (Uncle Fester's seems to be the
most logical) you'd have over 20 pounds of seeds to grind up and extract. 50,000
seeds. Thats a lot of seeds for 10 grams of LSA. Which would be 2 grams of LSD
assuming you got a 20% yield.
If you look into it further you can see that its really not .25% per seed, its 25% of all
alkoilds in the seeds.
"Alkaloid content of Hawaiian Baby Woodrose seeds
Ergine
22.68 0.136
Isoergine
31.36 0.188
Ergometrine
8.20 0.049
Lysergic alpha-OH-ethylamide
5.79 0.035
Isolysergic alpha-OH-ethylamide
3.98 0.024
The first number is the percentage of total alkaloid content and the second is
percentage of dry weight."
So each seed has .136 percent ergine/weight. So...
1 kilo of seeds... is 136mg of ergine, assuming perfect extraction with no impurites.
Times this by 5 kilos and you have 500mg. So even my 50,000 seeds assumption
isn't close.
Its just not possible.
A more simpler route is something such as ergocristine (what pickard used)
bromocristine (remove the bromo then convert) Paspalic acid, ergotamine, and some
other ergot chemicals that are much harder to convert..
Personally I've lost all hope to make LSD
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make it hard???
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That's actually the only reason I carry my weight around here. I don't know
chemistry and am not able to contribute from that perspective, but I can fucking read
and follow directions just fine and as a result I can get things going just because I
really really fucking want to despite my lack of knowledge (yeah I know, a disaster
waiting to happen lol).
I've reserved myself to just buying erogtamine tartrate. This is a very very viable
way for someone only interested in personal use amounts like myself. A box of 100
pills of Cafergot with a total of 100mg of ergotamine tartrate in them (100 pills times
1mg each) costs $60. With that 100mg of ergotamine extracted from them (not sure
how to do yet) you can get 30mg LSD. With that 30mg LSD you can get yourself 300
doses. Now what in the world does one need more then 300 doses for if he is not
interested in selling??? You can make a lifetime's supply off of one $60 box of
Cafergot!
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I just quickly sourced those and it wouldn't be a problem, but the erogtamine method
requires none of those or anything at all difficult to obtain. Taken from Tihkal:
SYNTHESIS : A solution of 6.7 g KOH in 100 mL H2O, under an inert atmosphere and
magnetically stirred, was brought to 75 C, and 10 g ergotamine tartrate (ET) added.
The reaction mixture turned yellow as the ergotamine went into solution over the
course of 1 h. The stirring was continued for an additional 3 h. The reaction mixture
was cooled to about 10 C with an external ice bath, and acidified to a pH of about
3.0 by the dropwise addition of 2.5 N H2SO4. White solids started to appear early in
the neutralization; approximately 60 mL of sulfuric acid was required. The reaction
mixture was cooled overnight, the solids removed by filtration, and the filter cake
washed with 10 mL Et2O. The dry solids were transferred to a beaker, suspended in
50 mL 15 % ammonia in anhydrous ethanol, stirred for 1 h, and separated by
decantation. This extraction was repeated, and the original decantation and the
second extract combined and filtered to remove a few hundred milligrams of
unwanted solids. The clear filtrate was stripped of solvent under vacuum, the residual
solids dissolved in 50 mL of 1% aqueous ammonia, and this solution was acidified as
before with 2.5 N H2SO4. The precipitated solids were removed by filtration and
washed with Et2O until free of color. After drying under vacuum to a constant weight,
there was obtained 3.5 g of d-lysergic acid hydrate, which should be stored in a dark,
sealed container.
A suspension of 3.15 g d-lysergic acid hydrate and 7.1 g of diethylamine in 150 mL
CHCl3 was brought to reflux with stirring. With the external heating removed, there
was added 3.4 g POCl3 over the course of 2 min, at a rate sufficient to maintain
refluxing conditions. The mixture was held at reflux for an additional 5 min, at which
point everything had gone into solution. After returning to room temperature, the
solution was added to 200 mL of 1 N NH4OH. The phases were separated, the
organic phase dried over anhydrous MgSO4, filtered, and the solvent removed under
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vacuum. The residue was chromatographed over alumina with elution employing a
3:1 C6H6/CHCl3 mixture, and the collected fraction stripped of solvent under hard
vacuum to a constant weight. This free-base solid can be recrystallized from benzene
to give white crystals with a melting point of 87-92 C. IR (in cm-1): 750, 776, 850,
937 and 996, with the carbonyl at 1631. The mass spectrum of the free base has a
strong parent peak at mass 323, with sizable fragments at masses of 181, 196, 207
and 221.
This base was dissolved in warm, dry MeOH, using 4 mL per g of product. There was
then added dry d-tartaric acid (0.232 g per g of LSD base), and the clear warm
solution treated with Et2O dropwise until the cloudiness did not dispel on continued
stirring. This opaqueness set to a fine crystalline suspension (this is achieved more
quickly with seeding) and the solution allowed to crystallize overnight in the
refrigerator. Ambient light should be severely restricted during these procedures. The
product was removed by filtration, washed sparingly with cold methanol, with a cold
1:1 MeOH/Et2O mixture, and then dried to constant weight. The white crystalline
product was lysergic acid diethylamide tartrate with two molecules of methanol of
crystallization, with a mp of about 200 C with decomposition, and weighed 3.11 g
(66%). Repeated recrystallizations from methanol produced a product that became
progressively less soluble, and eventually virtually insoluble, as the purity increased.
A totally pure salt, when dry and when shaken in the dark, will emit small flashes of
white light.
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two if every one tried it probably 90% would kill them selves and thouse near to
them.
becarefull but by all means if you can work it out and put the time and money into
doing it safely dont
let me stop you just shut your mouth when you get it right.
a note on doseage :)
truly if your to be an acid cat the print is a must as is belived by most of the acid
comunity.
it gives the cat an idea of what acid can do to some one and hopfully makes them
honorable and
reponsible in its use/missuse
acid can be very very dangerous if in the wrong hands.
prints are in the reagon of 1mg and up.
once you have been printed forget 100 mics working for you again well not for many
many years anyway.
30mg is not as much as it seems and once you have acid watch it disapear to every
one you know.
I belive the stuff should not be sold but given away.
but given only to the right people.
some people do not fair well on acid.
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There is probably another reaction which isn't harmful to the lysergic part.
Do you have an example of what is formed instead or any proper evidence?
I need more than just an incline to go on. ty
Quote from: shroomedalice on December 08, 2009, 07:49:15 AM
why dont you think the synth is just being given out by people and there are quite a few who do make
it to my knowlage.
one if every one had it in an open forum then kiss the shit goodbye as its number one on the bad lists
for the DEA
Who are you talking to? What questions are you answering?
Quote from: shroomedalice on December 08, 2009, 07:49:15 AM
I belive the stuff should not be sold but given away.
but given only to the right people.
Not true.
Thanks a bunch for the info, but mitragynine (from speciosa) is nothing to do with
ergoline (http://upload.wikimedia.org/wikipedia/en/thumb/2/2d/Mitragynine.png
/200px-Mitragynine.png)
(http://upload.wikimedia.org/wikipedia/commons/thumb
/8/80/Lysergic_acid_chemical_structure.png/180pxLysergic_acid_chemical_structure.png)
and a 'mild hydrolysis' isn't going to sort that. However, chromatography would be
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able to separate the LSA's; however I couldn't find any evidence anywhere of
speciosa containing any ergoline alkaloids, whatsoever.
help us out here... ?
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Or like was mentioned earlier, 10-20 boxes of those pills will get you to the same
place. I sort of like the romantic nature of "homespun" from those seeds to LSD...
After this treatment, how does one know which band is the winner? I know exactly
how one would test iso-lsd from lsd :), but LSA? Do both make you tired or just one?
HATU really looks like it rocks. After the other battles, that part actually is pretty
easy.
If one started with the correct LSA, the product should only need reXtal to a thing of
beauty if using HATU.
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Yeah I know the hydrazine hydrate method, from urea and sodium hypochlorite in a
gelatin matrix right?
But do enlighten us about the SO3. AFAIK that had to be ordered or was extremely
dangerous.
Although considering the circumstances hydrazine and conc. fuming SO3 we're talkin'
six and half a dozen! LOL
a lovely sip of burn your retinas off, anyone? :P
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Not true.
Thanks a bunch for the info, but mitragynine (from speciosa) is nothing to do with ergoline
(http://upload.wikimedia.org/wikipedia/en/thumb/2/2d/Mitragynine.png/200px-Mitragynine.png)
(http://upload.wikimedia.org/wikipedia/commons/thumb/8/80/Lysergic_acid_chemical_structure.png/180pxLysergic_acid_chemical_structure.png)
and a 'mild hydrolysis' isn't going to sort that. However, chromatography would be able to separate the
LSA's; however I couldn't find any evidence anywhere of speciosa containing any ergoline alkaloids,
whatsoever.
help us out here... ?
The speciosa I was referring to was Argyrea nervosa var speciosa i.e. the cheaper
variety of hbwr. Not Kratom:) I should have been explicit.
Argyrea nervosa var speciosa is what the cheaper sources in India sell. It isn't as
potent as the Hawaiian strain, nor are the effects as desirable. Its cheap though,
50/key. Like I said if there are any appreciable quantities of alkaloids this would be
viable at the price. I can assure you the speciosa variety contains ergot alkaloids,
the experience is not near as pleasant as morning glory seeds or hbwr from hawaii,
but unmistakably ergoline in nature.
The hydrolysis converts many of the alkaloids into lsa does it not? I've always read
to conduct the hydrolysis on the crude extract before running a column. If the
hydrolysis converts more of the alkaloids into the desired compound this is a logical,
yield maximizing step, no?
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ergot culture, or total synthesis are the only two real ways to go about it. I could be
wrong, but it seems here that its mostly going to be a big waste of time playing with
muddy solutions from ground seeds, etc.
Liquid Ergot culture is proper way. Steel tank drum for it is best to make solution. It
can become a test factory from being a scale up to a the greater amount. There is a
future in here.
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Understandable, I was just thinking that ergot would have more potential than HBWR
and should be considered and looked into, it might even be easier -- however, I
guess that is obvious, and this is also great to look more into this, as you never know
what you may come across. HBWR could be a pretty decent way, not that I have any
real interest in it.
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and possibly a respirator would be needed, but those are pretty simple to rig up.
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use solvent and base to extract the alkaloids i understand recovery is pretty efficient
and the hassle of rotovapping gallons of solvent is eliminated.
and production of pocl3 from p4o10 still requires phosphorous pentachloride not
exactly something that comes off a hardware store shelf and is probably watched
because of it's implications in nerve agents.
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What about a strong base hydrolyse of Ergive to give lysergic acid, and then let react
it with diethylamine hydrochloride ?
Is that normal that I bought pure Diethylamine hcl salts at my drugstore ? I was like
"uhhh what ? you really sell that ?". It that normal or only because I'm french ?
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solution of tartaric acid (saturated). the ammount needed is just enough to cover
the powder with 1cm of fluid and is allowed to stand cold for 24 hours in the dark.
more acidic methanol may be added as the seed powder absorbes it.
3.) after 24 hours the methanol is removed by vaccume to compleate dryness. the
seeds are then made into a slurry with DMF/DCM and loaded into a large column,
the DMF/DCM is allowed to drain through and more is added until test drops
evapurate with no residue. save the DMF/DCM filtate.
4.) the residual DMF/DCM is then removed by vaccume and the seed powder loaded
back into the column and filled with chilled MeOH and allowed to stand for 2hr before
draining. this is repeated 4 times and the methanol extracts combined, filtered and
reduced under vaccume to a small volume. cold ether is added to the methanol
solution
untill cloudiness does not dispell and is placed in a very cold fridge for the crystals to
set overnight. save this solution. this should afford 6-10g mixed LAA's as the
tartarate salt.
5.) the crystals are desolved in 200ml MeOH with 11g KOH and the methanol is
removed immediatly by vacuum as soon as the amide is desolved. the residue is
desolved in
200ml 8% KOH in DH2O and heated with a stream of nitrogen passed through it,
ammonia gas will be evolved and titrated with HCL to follow the reaction (HCl fumes
profusely in
the presence of ammonia gas). as soon as it is compleate cool the solution and slowly
add 2 or 3N sulfuric acid untill a PH of 3 is obtained, this will result in precipitation of
crude
D-lysergic acid monohydrate. save the solution.
6.) the crystals should be desolved in 200ml abs. EtOH containing a few ml of strong
ammonia (or gassed with anhydrous ammonia untill the solution has gained 3g) the
solids
that do not desolve within 1 hr are inorganic and can be discarded. filter the solution
through a column packed with 3in of 100 grit basic alumina/silica wetted with
anhydrous EtOH.
7.) the alcohol solution is again acidified with 2-3N sulfuric acid untill a PH of 3 is
obtained and is placed in the fridge overnight to crystalize. the crystals are filtered
out and dried
in a vaccume desicator or centerfuge. this will yeild 4g to 8g D-lysergic acid
monohytrate.
8.) there is still Iso-lysergic acid and amides in the solutions you saved. remove the
solvent in all three by vaccume using only heat from a hot water bath under 80*C.
desolve the
residues in a mixture of EtOH/MeOH 3:1 and combine. basify with a saturated
NaHCO3 solution and extract with ether or chloroform, remove the solvent by
vacuum and process
the residue through steps 5-7 for additional yeild.
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9.) desolve the crystals in abs. EtOH and THF 2:3 and process through a
chromatography column following the blue band with a weak long wave UV light.
collect that fraction and
remove the solvent by vaccume to get pure D-Lysergic acid monohydrate.
the D-LA should be cold stored -0*C in the absence of light and oxygen.
Diethylamine
make a solution of 60g KOH/NaOH (NaOH works better) in EtOH (50ml) its okay if it
dosent all dissolve. add 175ml DEET (98.11%) to this solution in an autoclavable
media bottle (can withstand high pressures) and place in a crockpot (sealed) set on
high. let it get to 80C and stay there for 1.5-2hr. over this time the solution will
progress from a clear soln to a dark piss yellow soln. after the 1.5-2hr remove and
cool the bottle before you open it or you'll spray diethylamine vapor everywhere.
fractionaly distill the solution with the addition of 20g lye to the distillation flask. the
diethylamine will come over at 55.5C (or 130F) the ethyl alcohol will come over at
78.4 C (or 173 F) the M-toluic acid dosent boil till about 230C so you wont be
distilling any of that or the lye over. since undoubtedly some of the EtOH and a little
water came over you will have to distill again but distill over NaOH (25g per 25ml of
distillate) and play close attention to the tempetures as the fractions start coming
over. the temp will continue to rise untill it hits the boiling point of the diethylamine
and stop there. when it starts to climb again all of the diethylamine is across and the
EtOH will start coming over nect would be the water if it didnt get trapped by the lye.
you can expect to get about 30g (or 90 ish ml) form 175ml of DEET, that is enough
for a few small batches as you only need about 7g per 3g of lysergic acid...
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im still working on the vacuum soxlet schematics now. but there would only be one
custom piece that would have to be made. that would consist of a large hopper/tank
made from stainless steel tubing (30x80cm about a 57L capacity) fitted with a
suitable head that has a valve and fritted discs for filters. it would essentialy be a
manual soxlet so it would have to be constantly watched while running but it would
allow you to process close to 100lbs of ergot/seeds at a time using only 5L or so of a
chloroform/methanol/ammonia mix. with vacuum from an aspirator applied you
would only need the heat from a hot water bath to drive the distillation.
as for the labware you would need: at least a 20L 2 or 3 neck flask, 400mm
graham/friedrich condenser, 400mm allihn condencer, vacuum adapter, tubing and
water aspirator vacuum probally totaling close to $300 and the hopper/tank i could
see coming close to $200 so mabey $500-600 over all which is chump change if you
are gonna process that much material and make LSD from it. just add a heating
mantle, 500ml flask and some rubber septums and you would also have every thing
needed to preform the synth its self.
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that much to go to hawaii in September. make some friends, find a big old hbwr vine
and ship seeds back in coffee bags. just make sure they are the foil lined ones and
vacuum seal them before you ship. a few weeks squating on the pipeline for free will
let you scroung up several KG pretty much for free (well you plane ticket S&H at
least). so now when you fly home you will have 10, 20 whatever kg you gathered in
your time there waiting for you. now you have something to work with, if you were to
go the hydrazide and POCl3 route 10kg might get you 10-15g....... now would that
be worth a $500 plane ticket?
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it should work the same exept sulfur chemistry is a bit quarky but i see no reason it
won't work.
except ergolines have that touchy conjugated double bond that lewis acids like zinc
acetate might influence and cause unwanted side reactions.
like dimerization for example because ergoline chemistry is a royal pain in the arse.
but if you got bromocryptine on hand give it a whirl.
it will only cost you a few quid to find out.
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