反应详情

2.6 g (8.40 mmol) of the above prepared [2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-acetic acid methyl ester in 15 ml of dry tetrahydrofuran was added under an argon atmosphere within 15 minutes to a stirred suspension of 0.38 g (10 mmol) of lithium aluminum hydride in 5 ml of tetrahydrofuran. The reaction was exothermic. Subsequently, the mixture was stirred at room temperature for 1 hour. Then, 1 ml of ethyl acetate was dropped to the reaction mixture, followed by water, drop after drop, under argon, with stirring and cooling until the gas evolution ceased. The reaction mixture was diluted with 50 ml of ethyl acetate, dried over anhydrous sodium sulfate, and filtered. The filtrate was evaporated i. V. and the residue was chromatographed on SiO2 with a mixture of dichloromethane and tert.-butyl methyl ether (4:1 vol./vol.) as eluent. Thereby, 1.88 g of the title compound was obtained as white solid.

1. stirringunder argon, with stirring
2. temperaturecooling until the gas evolution
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. customThe filtrate was evaporated i
6. customand the residue was chromatographed on SiO2 with a mixture of dichloromethane and tert.-butyl methyl ether (4:1 vol./vol.) as eluent