반응 #434821

반응 방정식

lithium aluminium hydride

2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one

ammonium hydroxide

→

2,3,4,5-Tetrahydro-1H-1,5-benzodiazepine

용매

THF

THF

THF

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도at reflux for 2 h
3. 3
   온도The mixture was then cooled to 0° C.
4. 4
   여과filtered through a pad of celite
5. 5
   기타The filtrate was evaporated in vacuo
6. 6
   기타to give a tan solid

실험 절차

To an ice cold solution of lithium aluminium hydride (4.68 g, 123 mmol) in dry THF (100 ml), under a nitrogen atmosphere, was added dropwise a solution of 2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one (5.0 g, 30.9 mmol) in dry THF (50 ml). The mixture was allowed to warm to room temperature and then heated at reflux for 2 h. The mixture was then cooled to 0° C. and a solution of aqueous ammonium hydroxide (10 ml) in THF (60 ml) was added dropwise. The resultant suspension was stirred for 1 h and then filtered through a pad of celite. The filtrate was evaporated in vacuo to give a tan solid; yield 4.36 g (95%).

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