反应详情

温度

60 °C

A solution of 7.2 g (22 mmol) of ethyl 2-(2,4,5-trifluoro-5-methylbenzoyl)-3-cyclopropylaminoacrylate in 100 mL of dry t-butanol was treated portionwise with 2.8 g (25 mmol) of potassium t-butoxide, and the reaction mixture was stirred at 60° C. for 5 hours. The suspension was cooled to room temperature and concentrated. The residue was partitioned between dichloromethane and 1N hydrochloric acid; the organic phase was washed with water, dried over magnesium sulfate, and concentrated. The crude product was slurried in boiling ethanol, filtered, and air-dried to give 4.2 g of the title compound.

1. temperatureThe suspension was cooled to room temperature
2. concentrationconcentrated
3. customThe residue was partitioned between dichloromethane and 1N hydrochloric acid
4. washthe organic phase was washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. filtrationfiltered
8. customair-dried