反应详情

A solution of 2,2-difluoroethanol (1.7 g; 20.6 mmol) in THF (50 mL) was added to a solution of ethyl 2-fluoro-4-(methylamino)-5-nitrobenzoate (5.0 g; 20.6 mmol) in DMF (100 mL). Sodium hydride (0.824 g; 60%; 20.6 mmol) was added in portions and the mixture was stirred over night at rt. A solution of TFA (30 mL; 0.45 M aq) was added and the mixture was concentrated. The resulting precipitation was filtered off, washed with water, dried and recrystallized from EtOH/water to give the sub-title compound. Yield: 4.8 g (76%).

1. concentrationthe mixture was concentrated
2. customThe resulting precipitation
3. filtrationwas filtered off
4. washwashed with water
5. customdried
6. customrecrystallized from EtOH/water