Reaktion #83486

Reaktionsgleichung

water

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

diborane dimethylsulfide

NaOH

→

colorless oil

Ausbeute 99.9%

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

Ausbeute 99.9%

Lösungsmittel

tetrahydrofuran

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is refluxed for 3 hours
2. 2
   SonstigeThe tetrahydrofuran is removed under vacuum
3. 3
   Extraktionthe residual aqueous mixture extracted with diethyl ether
4. 4
   WaschenThe extract is washed with brine
5. 5
   Trocknendried (Na2SO4)
6. 6
   Sonstigethe solvent removed

Vorschrift

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).

Quelle