反应详情

To a mixture of (cyanomethyl)triphenylphosphonium bromide (70.6 g, 185 mmol) and sodium hydroxide (7.39 g, 185 mmol) in DCM (100 mL) and water (300.00 mL) at 0° C. was added 3-bromo-4-fluorobenzaldehyde (25.0 g, 123 mmol). It was allowed to warm to room temperature and stirred for 2 h. The organic layer was separated, and the water layer was extracted with DCM twice. The combined organic phases were dried over Na2SO4 and concentrated to give a crude product, which was washed with diethyl ether. The residue was purified to give the title compound as a white solid (35 g, 88% yield). LCMS: rt=1.50 min, [M+H+]=226

1. customThe organic layer was separated
2. extractionthe water layer was extracted with DCM twice
3. dry with materialThe combined organic phases were dried over Na2SO4
4. concentrationconcentrated
5. customto give a crude product, which
6. washwas washed with diethyl ether
7. customThe residue was purified