反应详情

温度

-78 °C

To a solution of ethyl 2-(trifluoromethyl)pyrimidine-5-carboxylate (25.5 g, 116.0 mmol) in dichloromethane (580 mL) at −78° C. was slowly added DIBAL-H (1.0 M; 130.0 mL, 130.0 mmol). The mixture was stirred at −78° C. After 2 h, the mixture was quenched via slow addition of HCl (2.0 M in water). The mixture was allowed to warm to ambient temperature. The mixture was extracted with diethyl ether (3×). The combined organic extracts was dried over Na2SO4, filtered and concentrated to give the title compound (28.2 g).

1. customat −78° C.
2. customthe mixture was quenched via slow addition of HCl (2.0 M in water)
3. temperatureto warm to ambient temperature
4. extractionThe mixture was extracted with diethyl ether (3×)
5. dry with materialThe combined organic extracts was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated