Experiment Synthesis of Butyl Acetate
1. Aim of experiment
(1) Understood the basic synthesis principle and basic operation of organic acid ester
under acid catalysis.
(2)Master the basic operation of back flow dividing water, lavation, dryness and
distillation.
2．Principle of experiment
The main reaction:
O
O
+
H3C
H3C
OH
H3C
OH
O
CH3
The side eaction:
13
H3C
11
12
14
4
OH
10
H3C
5
2
3
6
O
8
7
1
CH3
9
3. Main apparatus and chemical reagents
Distillation flask, bulb condensation pipe, distillation conk, frank prolong, tail pipe,
three-mouth flask.
N- butyl alcohol, ice vinegar, concentrated sulfuric acid, soda solution, anhydr-sal
epsom, pH test paper.
4. Experiment procedures
(1) Back flow dividing water. 14.4mL acetic acid and 28.9mL alcohol are put into the
250mL distillation flask. The 10 drop concentrated sulfuric acid is put into the 250mL
distillation flask. Several zeolites are put into. Fit the bulb condensation pipe and
dividing water organ on the 250mL distillation flask. Put through condensate water.
Heat distillation flask until the liquid inside it refluxes about 40min.
(2) Divide the liquid and clean it. Cool when back flow end. Take the bulb
condensation pipe. The layer of ester from dividing water organ and reaction liquid
from three-mouth flask are put into separating funnel together. Clean with 20mL water.
Divide the layer of water.
(3) Remove acetic acid. Drip 25mL soda solution slowly into three-mouth flask which
can be gotten together distillation cut. The gas of CO2 is transgressed after rocking the
three-mouth flask continually. Check up the upper layer inside three-mouth flask with
litmus paper. Divide the layer of water when the upper layer isn’t red.
(4)Dryness. The layer of ester is put into dry conical flask. The anhydr-sal Epsom is
put into it. Desiccate it.
(5) Distillation and purification. The Butyl Acetate after dryness is shift to a dry 50mL
distillation flask. Fix distillation equipment with dry instrument. Several zeolites are
put into. Distill and get together the distillation cut between 124℃ and 126℃. Record
the boiling point of distillate in detail. Quantify the result and calculate rate of
production.
5. Matters need attention
(1) Tail water when the water refluxes into the reactive system.
(2) When the reaction go on about 40min and no sweat sink in the dividing water
organ, the reaction end.
6. Questions
(1) How do we get rid of water in the reaction?
(2) How to calculate the dividing water which can ensure reaction safe.