反应 #3665

反应方程式

water

6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one

diborane dimethylsulfide

NaOH

→

colorless oil

收率 99.9%

6,7-Dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine

收率 99.9%

溶剂

tetrahydrofuran

tetrahydrofuran

反应条件

后处理

1. 1
   温度The mixture is refluxed for 3 hours
2. 2
   其他The tetrahydrofuran is removed under vacuum
3. 3
   萃取the residual aqueous mixture extracted with diethyl ether
4. 4
   洗涤The extract is washed with brine
5. 5
   干燥dried (Na2SO4)
6. 6
   其他the solvent removed

实验过程

To a solution of 0.070 g of 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one in 2 ml of tetrahydrofuran is added 0.45 ml of a 2.0M solution of diborane-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 3 hours, poured into water and make basic with 2N NaOH. The tetrahydrofuran is removed under vacuum and the residual aqueous mixture extracted with diethyl ether. The extract is washed with brine, dried (Na2SO4) and the solvent removed to give 0.065 g of a colorless oil; one spot by thin layer chromatography (silica gel) with ethyl acetate-hexane (1:2) as solvent (Rf 0.81).

来源