反应详情

温度

0 °C

To a solution of 2-(3,4-dichlorophenyl)-2-methylpropanal (47.13 g, 0.217 mol) in Et2O (223 mL) at 0° C. was added a 3.0M solution of MeMgBr (217 mL, 0.651 mol) in Et2O. After stirring 2 h at 0° C., the reaction mixture was warmed to room temperature over 1 h. Then the reaction mixture was cooled to 0° C., quenched with H2O (100 mL) and 3N HCl (200 mL), extracted with EtOAc and washed with brine. The organic layer was dried over Na2SO4 and concentrated to afford the crude product, which was purified by column chromatography to yield 3-(3,4-dichlorophenyl)-3-methylbutan-2-ol (45.9 g, 90%). 1H NMR (400 MHz, CDCl3) δ 7.46 (d, 1H), 7.37 (d, 1H), 7.21 (dd, 1H), 3.83 (m, 1H), 1.31 (s, 3H), 1.29 (s, 3H), 1.05 (d, 3H).

1. temperaturethe reaction mixture was warmed to room temperature over 1 h
2. temperatureThen the reaction mixture was cooled to 0° C.
3. customquenched with H2O (100 mL) and 3N HCl (200 mL)
4. extractionextracted with EtOAc
5. washwashed with brine
6. dry with materialThe organic layer was dried over Na2SO4
7. concentrationconcentrated
8. customto afford the crude product, which
9. customwas purified by column chromatography