反应详情

温度

60 °C

To a mixture of 9.05 g (26.3 mmol) of ethyl 2-(2,3,4,5-tetrafluoro-5-methylbenzoyl)-3-cyclopropylaminoacrylate in 100 mL of dry t-butanol was added a slurry of 3.25 g (29.0 mmol) of potassium t-butoxide in 20 mL of dry t-butanol, and the mixture was stirred at 60° C. for 4 hours. The suspension was cooled to room temperature and concentrated to a paste which was partitioned between dichloromethane and 1N hydrochloric acid. The organic layer was separated, dried over magnesium sulfate, and concentrated. Recrystallization from ethyl acetate:hexane gave 4.70 g of the title compound, mp 176°-177° C.

1. temperatureThe suspension was cooled to room temperature
2. concentrationconcentrated to a paste which
3. customwas partitioned between dichloromethane and 1N hydrochloric acid
4. customThe organic layer was separated
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customRecrystallization from ethyl acetate