反应详情

温度

-78 °C

To a solution of 46.5 g (0.169 mol) of ethyl 4-(4-fluorophenyl)-2,6-dimethyl-5-pyrimidinecarboxylate in 500 mL of dichloromethane at -78° C. under nitrogen was added 340 mL of a 1M solution of diisobutylauminum hydride (0.339 mol) in dichloromethane. The resulting mixture was stirred at -78° C. for one-half hour and then the reaction was quenched by the addition of a saturated aqueous solution of sodium sulfate (48.15 g, 0.34 mol). The cooling bath was removed and the mixture was vigorously stirred for twenty minutes and then filtered through Celite®. The filter cake was thoroughly washed with chloroform and the combined filtrate and washings were dried over anhydrous magnesium sulfate and evaporated to yield 31.14 g of 4-(4-fluorophenyl)-2,6-dimethyl-5-pyrimidinemethanol, mp 174°-176° C.

1. customThe cooling bath was removed
2. stirringthe mixture was vigorously stirred for twenty minutes
3. filtrationfiltered through Celite®
4. washThe filter cake was thoroughly washed with chloroform
5. dry with materialthe combined filtrate and washings were dried over anhydrous magnesium sulfate
6. customevaporated