反应详情

N-[(t-Butyloxy)carbonyl]hydrazine (12 g) and 10 g of triethylamine were dissolved in 200 ml of dichloromethane and, at 0° C., 24 g of 2,3-bis(acetyloxy)benzoyl chloride in 50 ml of dichloromethane was added dropwise with stirring (30 minutes). After continuous stirring for one hour, the reaction mixture was extracted with 200 ml of ice water, 50 ml of 1% sodium bicarbonate and 100 ml of 5% citric acid. The organic phase was then washed with 100 ml of water, dried over sodium sulfate, and the solvent distilled off. The remaining oil crystallized after stirring with hexane. The result was beige crystals, 26.3 g; melting point 117° C.

1. stirringAfter continuous stirring for one hour
2. extractionthe reaction mixture was extracted with 200 ml of ice water, 50 ml of 1% sodium bicarbonate and 100 ml of 5% citric acid
3. washThe organic phase was then washed with 100 ml of water
4. dry with materialdried over sodium sulfate
5. distillationthe solvent distilled off
6. customThe remaining oil crystallized
7. stirringafter stirring with hexane