反应详情

温度

80 °C

In a mixture of 21.2 ml of t-butanol and 2.1 ml of water were dissolved 4.3 g of 4-cyanobenzoic acid t-butyl ester, 1.84 g of hydroxylamine hydrochloride and 2.31 g of sodium hydrogencarbonate. The solution was stirred for 2 hours at 80° C. To the reaction mixture was added water, and the mixture was subjected to extraction with ethyl acetate. The organic layer was concentrated under reduced pressure. The concentrate was purified by means of a silica gel column chromatography (hexane/ethyl acetate=1/1), followed by crystallization from hexane to afford 4.41 g of the titled compound as colorless needles.

1. extractionthe mixture was subjected to extraction with ethyl acetate
2. concentrationThe organic layer was concentrated under reduced pressure
3. customThe concentrate was purified by means of a silica gel column chromatography (hexane/ethyl acetate=1/1)
4. customfollowed by crystallization from hexane