反应详情

温度

50 °C

A suspension of 12.0 g (77.9 mmol) of 2-fluoro-4-hydroxyacetophenone, 27.9 g (85.6 mmol) of cesium carbonate and 11.6 ml (77.9 mmol) of ethyl 2-bromo-2-methylpropionate in 200 ml of DMF was heated at 50° C. for 3 days. Twice a day additional 12.7 g (38.9 mmol) of cesium carbonate and 5.8 ml (38.9 mmol) of ethyl 2-bromo-2-methylpropionate were added (total of 2.5 equivalent). The mixture was neutralized with aqueous 10% KHSO4 and extracted with ether (3×). The organic phases were washed with aqueous 10% KHSO4, aqueous 10% NaCl and dried over sodium sulfate. The crude product was purified by flash chromatography over silica gel with heptane/AcOEt 9:1 to 6:1, to give 16.7 g of the title compound as colorless oil.

1. extractionextracted with ether (3×)
2. washThe organic phases were washed with aqueous 10% KHSO4, aqueous 10% NaCl
3. dry with materialdried over sodium sulfate
4. customThe crude product was purified by flash chromatography over silica gel with heptane/AcOEt 9:1 to 6:1