Acetone → 4,4'-Diamino-6-cyanobenzanilide

関与物質

反応手順

350 ml of oleum (30% by weight) was cooled down below 0° C. using an ice bath, 99.6 g (0.368 mol) of 4,4'-diamino-6-carbamoyl benzanilide in a powder form was added below 5° C. with stirring. The stirring was continued to the next day, and the solution was neutralized by adding 1100 ml of NH4OH (28% by weight) already cooled down to -5° to 0° C. The solution was sufficiently washed to remove salt by filtering and washed with a small amount of warm ethanol and then dried in a vacuum oven at 80° C. The dried reactant which was mixed with by-products was extracted by soxlet and treated with the activated carbon and then ethanol was added to recrystallize in the mixture solvent (acetone:ethanol=1:1). The light yellow-scalelike crystal was filtered and dried in a vacuum oven at 80° C. The light yellow-scalelike crystal was extracted again by soxlet with acetone and treated with the activated carbon. And then the white-scalelike crystal obtained by recrystalling in the mixture solvent (acetone:ethanol=1:1) was dried in a vacuum oven at 80° C. (40 g of the raw material was obtained and the boiling point thereof was 250° to 251° C.).

情報源と証拠