反应详情

温度

2 °C

25 g (122 mmol) 1-(4-Trifluoromethoxy-phenyl)-ethanone were added to a suspension of 16.5 g (147 mmol) potassium-tert-butylate in 250 ml toluene. The suspension was cooled to 2° C. and 17.5 ml (147 mmol) ethyltrifluoroacetate were added within 15 min. The mixture was stirred at ambient temperature for 14 h, cooled to 2° C. and brought to pH 6 with 10% aqueous H2SO4. Twofold extraction with tert-butyl methylether was followed by washing of the combined extracts with brine/ice water 1/1 and drying of the organic layer over sodium sulfate. The solvent was removed under reduced pressure and the residue purified by flash chromatography (silica gel, dichloromethane) to give 30.5 g (102 mmol, 83%) of the title compound as red oil.

1. temperaturecooled to 2° C.
2. extractionTwofold extraction with tert-butyl methylether
3. washby washing of the combined extracts with brine/ice water 1/1
4. dry with materialdrying of the organic layer over sodium sulfate
5. customThe solvent was removed under reduced pressure
6. customthe residue purified by flash chromatography (silica gel, dichloromethane)