PROCEDURE

1. A 25 ml of 1-butanol and 20 ml of glacial ethanoic acid was added to a 250 ml round

bottom flask,
2. 2 ml of concentrated sulphuric acid was added and 2 to 3 boiling chips was placed in
the flask. A heating mantle was used to heat the flask.
3. The mixture was reflux slowly for about half an hour.
4. After reflux, the round bottom flask was cooled at room temperature.
5. The mixture was poured into 50 ml of cold distilled water and the crude ester was
separated by using separating funnel.
6. The crude ester was washed with another 50 ml of cold distilled water and the
separation process was repeated by using separating funnel.
7. The separation process was repeated by washing with 20 ml of saturated sodium
bicarbonate solution, NaHCO3. Stir thoroughly and vigorously to mix the liquid layers.
8. Finally, the crude ester was washed with 30 ml of distilled water and was separated.
9. A 5 g of anhydrous magnesium sulphate was added to the crude ester for 10
minutes.
10. The crude ester was filtered and proceed with distillation proceed. The pure ester
was collected at 120-127 ⁰C. the observation was reported and the percentage yield
of the product was calculated.

DISCUSSION

The reaction involve in this experiment is acid catalyzed reaction.The purpose of adding
concentrated sulphuric acid to the mixture is because Concentrated sulphuric acid is used as
a catalyst, and has a dual role: Speeds up the reaction. Acts as a dehydrating agent, forcing
the equilibrium to the right and resulting in a greater yield of ester.The reason why to heat
the mixture by reflux and not by direct heating is because reflux used to catalyze chemical
reactions. It also allows heating for a long without losing the volatile reactants and products.
Refluxing helps speed up chemical reactions without having it evaporate or explode. By
cooling the vapours before it escape the system, the apparatus is able to not only maintain a
constant volume of solution but also induce reactions. For preparation of saturated solution
of sodium bicarbonate, dissolve a lot of bicarbonate in a proportionally large amount of
water, and then distill it. The ethanoic acid and the sulfuric acid were separated from
the ester by adding sodium bicarbonate. The sodium bicarbonate is very effective in
removing acids from solutions. The carbonate ion reacts with the free H+ ions from the acid
to make carbonic acid which dissociates into carbon dioxide and water. Anhydrous
magnesium sulfate (MgSO4) is commonly used as a drying agent in organic chemistry. It is
typically used to dry the organic layer after an aqueous work-up. Anhydrous magnesium
sulfate is added to the wet organic layer and the resulting solid magnesium sulfate hydrate is
simply removed by filtration, providing a dry (anhydrous) organic filtrate. Anhydrous
magnesium sulfate (MgSO4) used to remove water in crude ester. In organic chemistry,
distillation is a powerful tool, both for the identification and the purification of organic
compounds. The boiling point of a compound is one of the physical properties used to
identify it. Distillation is used to purify a compound by separating it from a non-volatile or
less-volatile material. When different compounds in a mixture have different boiling points,
they separate into individual components when the mixture is carefully distilled. Chemical
equation for the preparation of butyl ethanoate written as below:

CONCLUSION

From this experiment, ester was successful produced from the acid catalyzed reaction
between an alcohol and a carboxylic acid. The product has the distinct “banana” smell-
which indicates the presence of esters.