反応 #3665

反応方程式

water

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

diborane dimethylsulfide

NaOH

→

colorless oil

収率 99.9%

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

収率 99.9%

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度The mixture is refluxed for 3 hours
2. 2
   その他The tetrahydrofuran is removed under vacuum
3. 3
   抽出the residual aqueous mixture extracted with diethyl ether
4. 4
   洗浄The extract is washed with brine
5. 5
   乾燥dried (Na2SO4)
6. 6
   その他the solvent removed

実験手順

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).

出典