反应详情

温度

75 °C

A mixture of 5-iodo-1-methyl-1H-pyrazole (8.00 g), 1-ethynyl-4-(trifluoromethyl)benzene (6.54 g), copper(I) iodide (110 mg), bis(triphenylphosphine)palladium(II) dichloride (1.35 g), triphenylphosphine (504 mg), triethylamine (8.00 mL) and dimethylformamide (70 mL) was stirred at 75° C. for 2 hours. Thereafter, the reaction solution was added to water, and the obtained mixture was then extracted with ethyl acetate. The organic layer was successively washed with water and a saturated saline, and was then dried over anhydrous magnesium sulfate, followed by vacuum concentration. The residue was purified by column chromatography (silica gel cartridge, hexane:ethyl acetate=85:15 to 75:25), so as to obtain the title compound (7.74 g) in the form of a yellow solid.

1. extractionthe obtained mixture was then extracted with ethyl acetate
2. washThe organic layer was successively washed with water
3. dry with materiala saturated saline, and was then dried over anhydrous magnesium sulfate
4. concentrationfollowed by vacuum concentration
5. customThe residue was purified by column chromatography (silica gel cartridge, hexane:ethyl acetate=85:15 to 75:25)