Cesium carbonate → HCID 69457704, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of 0.21 g (0.62 mmol) of crude 1-(2-fluoro-4-hydroxy-3-methyl-phenyl)-ethanone, 0.45 g (1.37 mmol) of cesium carbonate and 0.24 ml (1.25 mmol) of ethyl 2-bromo-2-methylpropionate in 5 ml of DMF was heated at 50° C. for 7 h. Additional 0.10 g (0.31 mmol) of cesium carbonate and 0.06 ml (0.31 mmol) of ethyl 2-bromo-2-methylpropionate were added and stirred at 50° C. for 11 h. The mixture was neutralized with aqueous 10% KHSO4 and extracted with ether (three times). The organic phases were washed with aqueous 10% KHSO4, aqueous 10% NaCl solution, dried (Na2SO4) and evaporated. The crude product was purified by flash chromatography over silica gel with n-heptane/AcOEt 95:5 to give 0.048 g of the title compound as yellow liquid.

Provenance & Evidence