反应详情

To a solution of lithium aluminum hydride in tetrahydrofuran (1M, 15.82 ml) and dry tetrahydrofuran (30 ml) was added aluminum chloride (2.10 g) in portions; with stirring. After 5 mins, 1,3,9,10,11,12-hexahydro-3-methyl-2H-quino[4,3,2-ef][1,4]benzoxazepin-2-one (4.24) was added, and the reaction mixture was stirred at room temperature for four hrs. Ethyl acetate (200 ml) and 10% sodium hydroxide solution (200 ml) were added. The organic phase was separated, dried over anhydrous magnesium sulfate, and concentrated. The residue was adhered to silica and flash chromatographed (5% triethylamine/toluene). The appropriate fractions were concentrated and the residue was triturated with diethyl ether to yield 2.48 g (62%) of product, mp 169°-170.5° C.

1. stirringthe reaction mixture was stirred at room temperature for four hrs
2. customThe organic phase was separated
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customchromatographed (5% triethylamine/toluene)
6. concentrationThe appropriate fractions were concentrated
7. customthe residue was triturated with diethyl ether