反应详情

To a stirred solution of 1-[6-(5-bromo-2-chloro-benzyl)-2,3-dihydro-benzo[1,4]oxazin-4-yl]-2,2,2-trifluoro-ethanone (8.6 g, 19.8 mmol) in ethanol (40 mL) was added NaBH4 (1.5 g, 39.0 mmol) portion wise and the reaction mixture was stirred overnight. Excess of NaBH4 was quenched by adding aq. NH4Cl, and ethanol was evaporated. The residue was partitioned between ethyl acetate and water, and the organic layer was separated, washed with brine (40 mL) and dried over sodium sulphate. Crude product obtained after evaporation of solvent was purified by silica gel column chromatography to furnish 6-(5-bromo-2-chloro-benzyl)-3,4-dihydro-2H-benzo[1,4]oxazine (6.1 g).

1. customExcess of NaBH4 was quenched
2. additionby adding aq. NH4Cl, and ethanol
3. customwas evaporated
4. customThe residue was partitioned between ethyl acetate and water
5. customthe organic layer was separated
6. washwashed with brine (40 mL)
7. dry with materialdried over sodium sulphate
8. customCrude product obtained
9. customafter evaporation of solvent
10. customwas purified by silica gel column chromatography