IN a 5-l. flask are placed 1 kg. of crystallized (hydrated) oxalic acid, 1.66 kg. of 95 per cent ethyl alcohol, and 1.33 kg. of carbon tetrachloride. The flask is then fitted with a fractionating column, I meter long, to which is attached a condenser and an automatic separator so arranged that the lighter liquid flows off to a receiver (Fig. 1). The heavier liquid flows through a tower of anhydrous potassium carbonate, and then returns to the reaction flask. The bottom of the tower is connected with a small separatory funnel through which any potassium carbonate solution, which flows from the solid in the tower, may be withdrawn from time to time. The mixture in the flask is slowly distilled. As soon as about 500 cc. of the lighter liquid has collected, it is placed in a fractionating apparatus and distilled, the material which boils up to 79'0 being collected separately. This fraction, which consists principally of alcohol, with a little carbon tetrachloride and moisture, is dried with potassium carbonate and returned to the reaction mixture. The higher fractions are redistilled. The above process is continued until the distillate no longer separates into two phases (about twenty-seven hours). The liquid in the flask is then distilled with the use of a column until the temperature of the vapor reaches 85'0; the residue is then distilled under reduced pressure, and the fraction which boils at 106-107/25 mm. is collected. The yield is 920-960 g. of a colorless liquid (80-84 per cent of the theoretical amount). 2. Notes Water, ethyl alcohol and carbon tetrachloride form a ternary mixture boiling at about 61'0. This vapor mixture, on condensation, separates into two phases; the heavier liquid consists of carbon tetrachloride and alcohol with only small amounts of water; the lighter liquid consists of approximately 65 per cent alcohol, 25 per cent water and 10 per cent carbon tetrachloride. By taking advantage of this fact, it is possible to conduct the esterification at a temperature so low that the ethyl hydrogen oxalate first formed does not decompose into ethyl formate and other products, as is the case when the customary methods of esterification are employed. The reaction may be carried out somewhat more expeditiously if the oxalic acid be dehydrated independently before it is mixed with the alcohol; indeed, it is also possible to remove the bulk of the water from the alcohol itself by a similar method, before mixing it with the oxalic acid. However, since water is formed during the esterification, little is gained by this procedure.