Introduction Ethyl acetate can be prepared from concentrated acetic acid and ethanol in presence of a strong acid (here, sulfuric acid). (If these precursors are not available, you may check out another text on how to purify ethyl acetate from nailpolish) See mechanism of esterification for more detail on reaction. See also some theory on esterification in methyl benzoate synthesis. Precursors in this synthesis may seem hard to get, but, not impossible. Here we will use 96% ethanol, homebrewed quality is sufficient. Acetic acid is a bit harder to get. I've seen 60% acetic acid in most photography and paint stores, 100% (glacial acetic acid) can be bought/ordered from places dealing with photography. Synthesis may be carried out with 60% acetic acid, logically, expecting much lower yields. Procedure Materials: Glacial acetic acid (CH3COOH) 100% Ethanol (CH3CH2OH) 96% Sulfuric acid (H2SO4) 96% Sodium carbonate Na2CO3 Calcium chloride CaCl2 Into a 500 ml round bottomed flask place 50 ml 96% ethanol and add carefully 50 ml 96% H2SO4, while stirring. Close flask with a stopper with two holes: one with a dropping funnel, the other with a bent pipe connected to a downward condenser leading into a receiving flask. Reaction flask is immersed into an oil-bath with maintained temperature at 140oC (with thermometer in oil). A mixture of 470 ml glacial acetic acid and 500 ml 96% ethanol is then added through the dropping funnel drop wise. The speed of addition should be about the same as the formation speed of distillate. Obtained distillate consists of ethyl acetate, ethanol and acetic acid (there also forms diethyl ether and H2SO3). Ethyl acetate is separated by shaking distillate several times with a concentrated solution of sodium carbonate or calcium chloride (Note 1). Upper layer is separated in a separating funnel and dried by prilled calcium chloride. After filtering, dry product is fractionated collecting fraction of 72-78oC. Yield is 90% (Note 2). Notes 1. Washing product with both solution of sodium carbonate and calcium chloride should give better results. Distillate is first neutralised by sodium carbonate solution (150 g in 400 ml water) and then shaken twice with 200 ml portions of 50% CaCl2 solution. With primary alcohols, CaCl2 builds crystalline compounds, in this case CaCl2*2CH3CH2OH. Since this compound is not soluble in ethyl acetate and soluble in water, it's removed effectively. 2. I've tested this synthesis on 10 times smaller scale obtaining yields around 64%. The low yield could be explained by loss in downscaling. Anyway, 90% could be simply a typo in the book since yields from 3 other books lies in range of 65-67%. References 1. Preparation of synthetic chemo-pharmauceutic substances" M.M.Kacnelson 2:nd ed. 1923.