反应详情

温度

-10 °C

Methyllithium (1.3 M in diethyl ether, 35 mL) was added dropwise to 3-bromo-5-fluorobenzoic acid (5 g) in diethyl ether at −78° C. keeping the temperature below −60° C. The reaction was then left to warm to −10° C. and was stirred for 1 h before being carefully quenched with saturated ammonium chloride (100 mL) until pH=3. The product was extracted with diethyl ether (2×100 mL), dried over sodium sulfate and the solvent removed by evaporation to yield 1-(3-bromo-5-fluorophenyl)ethanone as an off-white solid (4.67 g, 94%). 1H NMR (CDCl3): 2.59 (3H, s, ArCOCH3), 7.44 (1H, dd, Ar), 7.59 (1H, dd, Ar), 7.87 (1H, s, Ar).

1. customthe temperature below −60° C
2. waitThe reaction was then left
3. custombefore being carefully quenched with saturated ammonium chloride (100 mL) until pH=3
4. extractionThe product was extracted with diethyl ether (2×100 mL)
5. dry with materialdried over sodium sulfate
6. customthe solvent removed by evaporation