反应详情

To a solution of lithium aluminum hydride in tetrahydrofuran (1M, 10.0 ml) and dry tetrahydrofuran (30 ml) was added aluminum chloride (1.86 g) in portions, with stirring. The reaction mixture was stirred for five mins and 1,3-dimethyl-1,3,9,10,11,12-hexahydro-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one (3.95 g) was added. After stirring for 30 min, ethyl acetate (200 ml) and 10% sodium hydroxide solution (200 ml) were added, and the organic layer was separated, dried over anhydrous magnesium sulfate and concentrated. Recrystallization of the residue from diethyl ether/pentane gave 2.2 g (59%) of product, mp 125°-126.5° C.

1. stirringThe reaction mixture was stirred for five mins
2. stirringAfter stirring for 30 min
3. customthe organic layer was separated
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customRecrystallization of the residue from diethyl ether/pentane