反应详情

温度

-70 °C

A mixture of 2-chloro-4-(trifluoromethyl)pyrimidine-5-carbonyl chloride (2.8 g) and dichloromethane (56 mL) was cooled in a dry ice-acetone bath, and morpholine (990 μL) and triethylamine (1.9 mL) were added dropwise thereto while keeping the temperature at −50° C. or lower. The reaction mixture was stirred at −70° C. for 2.5 hours, and then ethyl acetate and water were added thereto. The aqueous layer was extracted with ethyl acetate, and the organic layer was washed with water and saturated brine. After drying over anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate) to obtain 4-{[2-chloro-4-(trifluoromethyl)pyrimidin-5-yl]carbonyl}morpholine (2.8 g) as a white solid.

1. temperaturewas cooled in a dry ice-acetone bath
2. customat −50° C.
3. extractionThe aqueous layer was extracted with ethyl acetate
4. washthe organic layer was washed with water and saturated brine
5. dry with materialAfter drying over anhydrous magnesium sulfate
6. customthe solvent was evaporated under reduced pressure
7. customthe obtained residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate)