MAKING METH

Notes: Initial chemical reaction could take 24 to 36 hours Yield is about 100% less 50% l-Meth which is recycled Highest yield is obtained when lowest possible temperature is used Temperature should be worked up to, as amount and quality depends on it N-Methylformamide ready made will have to be distilled under a vacuum first before using in this reaction. Avoid water at all costs during P2P/N-Methylformamide reaction.

Equipment: Round bottom flasks Sep funnel Claisen adapter Stillhead Stoppers Vacuum adapt er Vacuum pump or aspirator Hot Plate Metal bowl for oil bath 2 x Thermometers Boiling chips Retort stands for suspension of flasks Long and short condensers Bent piece of glass tubing to join condensers

Chemicals, etc: P2P N-Methylformamide Formic acid (88%) Lye HCl acid (35% lab grade) Toluene Distilled water Ice and tap water for condensers Oil for oil bath

Test Chemicals: - 5ml P2P and 10ml N-Methylformamide in clean dry glass container (Within a few seconds the chemicals should mix together entirely)

Reaction Procedure: (Setup equipment as per the diagram below)

- In a 500 ml round bottom flask mix 100ml P2P, 250ml N -Methyl formamide and a small amount of Formic Acid - Place flask in oil bath (Oil should cover 2/3 of flask remember that oil will expand when heated) - Low heat setting is applied until oil bath is 100 degrees over a 45 minute period - Contents of flask is stirred regularly with thermometer

- Temperature is slowly worked up to 105 degre es and contents stirred every 15 minutes (Temperature may need to go as high as 110 degrees until reaction starts) - Keep temperature at same level as when bubbling started until the reaction has almost stopped (Generally takes a couple of hours) - Raise temperature about 3 degrees and stir contents every 30 minutes - Keep raising temperature after reaction almost stops to get reaction going again until 140-145 degrees is reached and reaction stops (Reaction could take a long time between 120-130 degrees and in total up to 24-36 hours) - Heat is turned off when reaction stops and contents are allowed to cool (It should look like beer and without a reddish tint)

N-Methylformamide Recovery: (Setup equipment as per the diagram below)

- In a 2000ml round bottom flask mix 180g Lye is added to 450ml of distilled water - Once cooled add 5 boiling chips and add reaction mixture and swirl - Heat source is turned on to 1/3 maximum - The flow of ice water through long condenser is begun - Heat is turned down a little when boiling chips float between the Lye and the reaction mixture and some bubbling and frothing of reaction mixture begins - After reaction has subsided and bubbling of Methylamine into the Formic Acid has slowed down, heat to 2000ml flask is increased to maintain a good rate of Methylamine flow to the Formic Acid (Flask must not be heated so strongly that water is forced through glass tubing) - When Methylamine no longer flows evenly into the Formic Acid the heat is turned off and the level of Formic Acid flask is lowered so acid is not sucked back into the other flask (This Formic Acid is half reacted with Methylamine. Pour into a glass bottle and keep in freezer for production of N-Methylformam ide)

Acid/Base Extraction: (Reaction Mixture is about 100ml, has a red colour and floats above Sodium Hydroxide solution) - Once cooled contents of flask is poured into a 1000ml sep funnel - Sodium Hydroxide solution is drained out and thrown away - Red mixture is poured into 500ml flask with 3 boiling chips - 200ml HCl Acid is poured into sep funnel, swirled and then poured into 500ml flask (Setup equipment as per the diagram below)

- Gently boil 500ml flask for 2 hours (Mixture quickly turns black) - Turn off heat after 2 hours and let it cool down - In 1000ml flask mix 80g Lye and 250ml Distilled Water (If 35% lab grade HCl Acid was used in last step use 100g Lye and 300ml Distilled Water) - When both flasks have cooled the black mixture is cautiously added to the Lye solution (Add small portions and swirl to mix then stop to cool) - After all of black mixture has been added, the 1000ml flask is stoppered and shaken vigorously for 5 minutes - Add 1 00ml Distilled Water and swirl for a few minutes to dissolve salt crystals in bottom of flask (Add another 100ml of Distilled Water if all does not dissolve) - Once cooled pour into 1000ml sep funnel and add 100ml toluene - Sep funnel is stoppered and shaken for 15 seconds - Let it stand for a couple of minutes and then drain lower water layer into glass container - Brown Meth Toluene layer is poured into a clean dry 500ml flask - The water layer is extracted once more with 100ml Toluene then thrown away - The Toluene layer is poured into 500ml flask

Distillation: (Setup equipment as per the diagram below)

- Add 3 boiling chips to 500ml flask - Turn on heat to 1/4-1/3 maximum until mixture begins to boil - Increase heat until Toluene comes over (Pure Toluene should come over at 110 degrees) - Increase temperature in very small increments to keep toluene coming over - When temperature reaches 115 degrees or rate of Toluene collecting slows to a crawl, turn off heat and let flask cool down (Collected Toluene is poured into bottle to be used next time) (If foam is encountered whilst distilling off Toluene, turn on water to aspirator at a slow rate. Then vacuum hose is attached to the vacuum adapter and a weak vacuum is produced inside the glassware. Every few seconds the vacuum hose is removed, then reattached. The Toluene after a little while should begin to boil normally and the vacuum can be left off) - Apply vacuum to glassware at full strength - Last remnants of Toluene begin to boil and heat is turned back on to 1/3 maximum (If aspirator is being used, when temperature reaches 80 degrees the vacuum hose is quickly removed and the 250ml flask is replaced with a clean dry one. If using a good vacuum pump, make change at 70 degrees. Flask change is done quickly to avoid overheating in the distilling flask) - Meth distils over. Once distilled, turn off heat and disconnect vacuum (With aspirator, Toluene collects from 80-150 degrees depending on the strength of the vacuum. With vacuum pump it collects to about 120-130 degrees) (Product should be 90ml of clear to pale yellow freebase meth)

Separation of Isomers: - 85 parts of racemic methamphetamine are introduced into a solution of 100 parts of d-tartaric acid in 1000 parts of methyl alcohol - After a lengthy amount of time standing?, 100 parts of the precipitated salt are aspirated off (removed) and extracted with hot ethyl alcohol. (Since the d-tartrate of d-meth is readily soluble in both methyl and hot ethyl alcohol whereas the dtartrate of l-meth is sparingly soluble both in methyl and hot ethyl alcohol a simple separation of the d-tartrates of the base is effected)

Oxidize L-Meth to P2P: ??????????? (potassium permanganate)

Crystallization: - Evaporate slowly OR - Freebase Meth is dissolved in 2-3 volumes of Dry Acetone - Concentrated HCl Acid (35%) is added to the Dry Acetone whilst stirring until the pH is 4 or lower - HCl Acid is then precipitated from solution by slowly adding Toluene with stirring (It will take the addition of 10-20 volumes of Toluene to fully precipitate the HCl Acid) - Crystals are filtered out with about 15ml x 2 of Dry Acetone and set aside to dry (Filtrate could be tested for completeness of precipitation by adding some more Toluene to it) (Can be dried under vacuum attach vacuum hose to filtering flask and cover funnel with palm or section of latex glove. The vacuum builds and removes most of the solvent from the filtered crystals within about 60 seconds. See diagram below)

Recystal l ization: - Place impure solid on glass dish and add a small volume of hot dry Isopropyl (Add only enough hot dry alcohol to dissolve the solid and heat as needed) Filter solution

- Bring solution to a soft boil - Continue boiling until you begin to see the crystals on the surface of the alcohol - Turn off heat and add a little Isopropyl to dissolve the skin (crystals on surface) Set aside to cool slowly to room temperature - Add 20ml of ice cool dry Acetone (If it turns cloudy add dry alcohol dropwise until it is clear again) - Cover and place in freezer for 6 hours or more (The longer in the freezer, the bigger and better will be the crystals) - Then air dry with cool shot on hair dryer OR - Can be dried under vacuum attach vacuum hose to filtering flask and cover funnel with palm or section of latex glove. The vacuum builds and removes most of the solvent from the filtered crystals within about 60 seconds. OR - Dissolve crystals in the smallest amount of warm dry Isopropyl to dissolve them Filter solution

- Add 20x that volume of Toluene - After vigorous shaking for 3 minutes, crystals reappear (If not, more Toluene is added followed by more shaking) - Cover and place in freezer for 6 hours or more - Then air dry with cool shot on hair dryer OR - Can be dried under vacuum attach vacuum hose to filtering flask and cover funnel with palm or section of latex glove. The vacuum builds and removes most of the solvent from the filtered crystals within about 60 seconds.

Dry Isopropyl/Acetone: - Bake 25% Epsom Salts in oven at 200 degrees for an hour or until Epsom Salts makes a solid - Pour 75% Isopropyl/Acetone through filter with Epsom Salts mass