反应详情

A solution of ethyl-2-(10H-phenoxazin-10-yl)acetate (5.5 g, 20.44 mmol) in dry tetrahydrofuran (20 ml) was added dropwise to a suspension of lithium aluminum hydride (1.16 g, 30.52 mmol) in dry tetrahydrofurane (20 ml) at 0° C. The reaction mixture was warmed to room temperature and stirred for additional 1 h. The excess lithium aluminum hydride was quenched with a solution of saturated sodium sulfate at 0° C. The reaction mixture was filtered and the residue was washed with hot ethyl acetate (2×75 ml). The combined organic layers were dried (Na2SO4), filtered and the solvent was evaporated under reduced pressure to afford the title compound (4.6 g, 99%) as a colourless solid. The compound is used in the next step without further purification. mp: 113-115° C.

1. customThe excess lithium aluminum hydride was quenched with a solution of saturated sodium sulfate at 0° C
2. filtrationThe reaction mixture was filtered
3. washthe residue was washed with hot ethyl acetate (2×75 ml)
4. dry with materialThe combined organic layers were dried (Na2SO4)
5. filtrationfiltered
6. customthe solvent was evaporated under reduced pressure