反应详情

温度

-60 °C

To a stirred solution of ethyl fluoroacetate (0.33 ml; 3.3 mmol) in dry diethyl ether (3.3 ml) under argon at −76° C. was added dropwise a 0.25 M solution of 2,4-dichlorobenzylmagnesium chloride in diethyl ether (20 ml; 5 mmol). The suspension was stirred at −60° C. during 5 h. The mixture was poured in ammonium chloride sat. solution and extracted three times with diethylether. Organics were combined, dried over sodium sulfate and evaporated to a resin which was subject to flash chromatography (eluant: c-hexane/ethyl acetate 99:1 to 70:30) to afford 0.36 g (49% of theory) of 1-(2,4-dichloro-phenyl)-3-fluoro-propan-2-one as a pale yellow solid (melting point: 48-52° C.).

1. extractionextracted three times with diethylether
2. dry with materialdried over sodium sulfate
3. customevaporated to a resin which