反应详情

To the suspension of lithium aluminium hydride (15.2 g, 0.4 mol) in 600 mL of ether was added a solution of 4,5-dihydro-1,4-benzoxazepin-3(2H)-one (16.3 g, 0.1 mol) in 60 mL of tetrahydrofuran at room temperature. After being heated with stirring under reflux overnight, water was added dropwise to quench the reaction at 0° C., The resulting mixture was diluted with ethyl acetate, and then filtered by a pad of celite. The filtrate was concentrated under reduced pressure, followed by the addition of hydrochloric acid ethyl acetate solution. The hydrochloride was collected by filtration, washed with ethyl acetate then ether, and then dried in vacuo to give 13.5 g of product. MS obsd. (ESI+) [(M+H)+] 150.

1. temperatureAfter being heated
2. temperatureunder reflux overnight
3. customto quench
4. customthe reaction at 0° C.
5. filtrationfiltered by a pad of celite
6. concentrationThe filtrate was concentrated under reduced pressure
7. additionfollowed by the addition of hydrochloric acid ethyl acetate solution
8. filtrationThe hydrochloride was collected by filtration
9. washwashed with ethyl acetate
10. dry with materialether, and then dried in vacuo