반응 #3665

반응 방정식

water

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

diborane dimethylsulfide

NaOH

→

colorless oil

수율 99.9%

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

수율 99.9%

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   온도The mixture is refluxed for 3 hours
2. 2
   기타The tetrahydrofuran is removed under vacuum
3. 3
   추출the residual aqueous mixture extracted with diethyl ether
4. 4
   세척The extract is washed with brine
5. 5
   건조dried (Na2SO4)
6. 6
   기타the solvent removed

실험 절차

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).

출처