反应详情

A mixture consisting of 500 mg (1.54 mmol) of the 7-chloro-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one prepared in Step B of Example 1; 45.0 mg (0.15 mmol) of 2-(di-t-butylphosphino)biphenyl; 17.0 mg (0.075 mmol) of palladium acetate; and 713 mg (7.42 mmol) of sodium t-butoxide, was suspended in 15 ml of toluene. Thereafter, 0.533 ml (6.39 mmol) of pyrrolidine was added to the above suspension, and the obtained mixture was then stirred under heating to reflux for 2 hours. Thereafter, the reaction solution was stood to cool, and water was then added thereto, followed by extraction with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and was then concentrated. The obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5), so as to obtain 277.9 mg (50%) of 7-pyrrolidin-1-yl-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one in the form of a yellow solid.

1. temperatureunder heating
2. temperatureto reflux for 2 hours
3. temperatureto cool
4. extractionfollowed by extraction with ethyl acetate
5. dry with materialThe extract was dried over anhydrous sodium sulfate
6. concentrationwas then concentrated
7. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:5)