反应详情

温度

47.5 °C

3-Bromo-2-methylbenzonitrile (810 mg, 4.13 mmol) was stirred in THF (5 mL) at 0° C. under argon, and methylmagnesium bromide (1.6 mL, 4.8 mmol) (3.0 M solution in Et2O). The reaction was stirred at 45-50° C. for 2 h. The reaction was cooled to 0° C. and 6 N HCl (5 mL) was added carefully. The reaction mixture was stirred at 40-50° C. for 2 h. After cooling, the mixture was extracted with Et2O (2×). The organic layers were washed with H2O, brine, dried over MgSO4, filtered and concentrated to give Intermediate 12A (600 mg, 2.82 mmol, 68.2% yield) as yellowish oil. LCMS=1.27 min [M+1]=211.9, 213.9 (Method B).

1. temperatureThe reaction was cooled to 0° C.
2. stirringThe reaction mixture was stirred at 40-50° C. for 2 h
3. temperatureAfter cooling
4. extractionthe mixture was extracted with Et2O (2×)
5. washThe organic layers were washed with H2O, brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated