反应详情

To a cold (5° C.) solution of 2.77 g (6.64 mmol) of ethyl 3-(2,4-difluoroanilino)-2-(2,3,4,5-tetrafluoro-6-methylbenzoyl)acrylate in 60 ml of dry THF was added 0.32 g of 60% sodium hydride. The solution was stirred overnight at room temperature, then concentrated to an orange foam. The residue was partitioned between methylene chloride and 1N HCl. The organic phase was washed with water, dried over magnesium sulfate, and concentrated to an orange solid which was recrystallized (ethyl acetate:hexane) to give 1.55 g of the title compound, mp 152°-154° C.

1. concentrationconcentrated to an orange foam
2. customThe residue was partitioned between methylene chloride and 1N HCl
3. washThe organic phase was washed with water
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated to an orange solid which
6. customwas recrystallized (ethyl acetate:hexane)