반응 #1827198

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 2.0 M solution of diborane-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 3 hours, poured into water and make basic with 2 N 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