Acid Acetic Glacial, 96 per cent

The tests to be made are those given under Acid Acetic, Glacial, 96 per cent, observing the conditions there described. 

The tests to be made are those given under Acid Acetic, Glacial, 96 per cent, observing the conditions there described. But instead of 10 gm. of the 96 per cent, use 30 gm. of the 30 per cent. 

Ethyl isobutyrylisobutyrate. Add 24-6 g. (28-3 ml.) of ethyl iso-butyrate, b.p. 110-111°, to the solution of ca. 0 21 mol of sodium triphenyl-methide in approximately 1400 ml. of ether contained in the 2-litre conical flask. Stopper the flask, shake well to effect complete mixing, and keep at room temperature for 60 hours. Acidify the reaction mixture by adding, with shaking, 15 ml. of glacial acetic acid, and then extract with 100 ml. of water. Wash the ethereal solution with 50 ml. portions of 10 per cent, sodium carbonate solution until free from excess acid, dry over anhydrous magnesium sulphate, and distil off the ether on a steam bath. Distil the residue under reduced pressure from a Claisen flask with fractionating side arm (Figs. II, 24, 4—5). Collect the ethyl isobutyryl isobutyrate at 95-96°/18 mm. the yield is 15 g. The b.p. at atmospheric pressure is 201-202°. 

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