反应详情

A suspension of 4-bromobenzamide (9.50 g, 47.5 mmol) in 1,1-dimethoxy-N,N-dimethylmethanamine (17.2 mL, 47.5 mmol) in a round bottom flask topped with a short path distillation head was placed in a preheated sand bath at 122° C. The reaction mixture was allowed to stir at this temperature for 1.5 hours, during which time the MeOH that was formed was collected from the distillation condenser. Upon cooling solids were formed and collected by vacuum filtration affording (E)-4-bromo-N-((dimethylamino)methylene)benzamide as a pale yellow solid (9.38 g, 77%) which was used directly in the next step without further purification. LCMS (APCI+) m/z 255, 257 [M+H]+.

1. distillationtopped with a short path distillation head
2. customwas placed in a preheated sand bath at 122° C
3. customwas formed
4. distillationwas collected from the distillation condenser
5. temperatureUpon cooling solids
6. customwere formed
7. filtrationcollected by vacuum filtration