反应详情

温度

-78 °C

To a solution of 5-bromopyrimidine-2-carbonitrile (300 mg, 1.63 mmol) in THF (20 mL) was added MeMgBr (5.43 mL, 16.3 mmol) at −78° C. under nitrogen. The solution was stirred at −78° C. for 20 min., quenched with satd aq NH4Cl, and extracted with EtOAc. The combined organic layer was dried over anhydrous Na2SO4 and concentrated to give an oil, which was purified by prep TLC (3:1 PE/EtOAc) to give 1-(5-bromopyrimidin-2-yl)ethanone (99 mg, yield 30.2%). 1H NMR (CDCl3): δ2.70 (s, 3H), 8.90 (m, 2H).

1. customquenched with satd aq NH4Cl
2. extractionextracted with EtOAc
3. dry with materialThe combined organic layer was dried over anhydrous Na2SO4
4. concentrationconcentrated
5. customto give an oil, which
6. customwas purified by prep TLC (3:1 PE/EtOAc)