Reacción #3665

Ecuación de reacción

water

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

diborane dimethylsulfide

NaOH

→

colorless oil

Rendimiento 99.9%

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

Rendimiento 99.9%

Disolventes

tetrahydrofuran

tetrahydrofuran

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe mixture is refluxed for 3 hours
2. 2
   OtroThe tetrahydrofuran is removed under vacuum
3. 3
   Extracciónthe residual aqueous mixture extracted with diethyl ether
4. 4
   LavadoThe extract is washed with brine
5. 5
   Secadodried (Na2SO4)
6. 6
   Otrothe solvent removed

Procedimiento

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).

Fuente