反应详情

15.6 g of 8-bromo-3,4-dihydro-1-benzothiepin-5(2H)-one were dissolved in 70 ml of diethylene glycol. The solution was treated with 6.55 ml of hydrazine hydrate and 7.5 g of solid potassium hydroxide and heated to 180°-190° C. under reflux for about 30 hours. After cooling, the mixture was poured on to ice and extracted with ether. The organic phase was washed with water, dried and evaporated. Chromatography on silica gel with petroleum ether yielded 10.7 g of 8-bromo-2,3,4,5-tetrahydro-1-benzothiepine as a colorless oil.

1. temperatureheated to 180°-190° C.
2. temperatureunder reflux for about 30 hours
3. temperatureAfter cooling
4. additionthe mixture was poured on to ice
5. extractionextracted with ether
6. washThe organic phase was washed with water
7. customdried
8. customevaporated