反应详情

温度

100 °C

A suspension of 4-bromo-2-fluorobenzamide (0.929 g, 4.26 mmol) in 1,1-dimethoxy-N,N-dimethylmethanamine (1.66 mL, 11.7 mmol) in a round bottom flask topped with a short path distillation head was heated to 100-100° C. The resulting solution was allowed to stir at this temperature for 3.5 hours, during which time the MeOH that was formed was collected from the distillation condenser. Heptane (5 mL) was added dropwise and the resulting suspension was cooled to 0-5° C. The solids were collected by vacuum filtration, rinsed with excess heptane, and dried to afford (E)-4-bromo-N-((dimethylamino)methylene)-2-fluorobenzamide (1.111 g, 96%) as an off-white solid which was carried on without further purification.

1. distillationtopped with a short path distillation head
2. customwas formed
3. distillationwas collected from the distillation condenser
4. additionHeptane (5 mL) was added dropwise
5. temperaturethe resulting suspension was cooled to 0-5° C
6. filtrationThe solids were collected by vacuum filtration
7. washrinsed with excess heptane
8. customdried