تفاعل #3665

معادلة التفاعل

water

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

diborane dimethylsulfide

NaOH

→

colorless oil

المردود 99.9%

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

المردود 99.9%

المذيبات

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is refluxed for 3 hours
2. 2
   أخرىThe tetrahydrofuran is removed under vacuum
3. 3
   استخلاصthe residual aqueous mixture extracted with diethyl ether
4. 4
   غسيلThe extract is washed with brine
5. 5
   تجفيفdried (Na2SO4)
6. 6
   أخرىthe solvent removed

الإجراء التجريبي

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).

المصدر