反应详情

To 15 ml of formic acid was added dropwise 5 ml of acetic anhydride, and the mixture was stirred for 20 minutes at room temperature. To the mixture was added dropwise a solution of 2.2 g of 2,3,4,5-tetrahydro-1,4-benzoxazepine in 10 ml of dichloromethane, and the mixture was stirred for 30 minutes at room temperature. The reaction mixture was poured into ice-water, then the mixture was subjected to extraction with dichloromethane. The extract was washed successively with a saturated aqueous solution of sodium bicarbonate, and water. The mixture was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to give 2.6 g of 4-formyl-2,3,4,5-tetrahydro-1,4-benzoxazepine as an oily anhydrous substance.

1. stirringthe mixture was stirred for 30 minutes at room temperature
2. extractionthe mixture was subjected to extraction with dichloromethane
3. washThe extract was washed successively with a saturated aqueous solution of sodium bicarbonate, and water
4. dry with materialThe mixture was dried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure