반응 #65694

반응 방정식

8-bromo-3,4-dihydro-1-benzothiepin-5(2H)-one

hydrazine hydrate

potassium hydroxide

→

8-bromo-2,3,4,5-tetrahydro-1-benzothiepine

수율 72.5%

용매

diethylene glycol

반응 조건

후처리

1. 1
   온도heated to 180°-190° C.
2. 2
   온도under reflux for about 30 hours
3. 3
   온도After cooling
4. 4
   workup.ADDITIONthe mixture was poured on to ice
5. 5
   추출extracted with ether
6. 6
   세척The organic phase was washed with water
7. 7
   기타dried
8. 8
   기타evaporated

실험 절차

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.

출처