反应详情

Sodium methoxide (28% methanol solution, 69.1 g) was added to a solution of 4-bromo-2,3-difluorobenzaldehyde (52.8 g) in methanol (600 mL) at room temperature. The mixture was refluxed under nitrogen atmosphere for 2 hours and concentrated in vacuo to about 1/4 volume. The mixture was diluted with ethyl acetate and water. The mixture was extracted with ethyl acetate. The organic layer was separated, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title compound (52.3 g).

1. temperatureThe mixture was refluxed under nitrogen atmosphere for 2 hours
2. concentrationconcentrated in vacuo to about 1/4 volume
3. additionThe mixture was diluted with ethyl acetate and water
4. extractionThe mixture was extracted with ethyl acetate
5. customThe organic layer was separated
6. washwashed with water and brine
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated in vacuo