反应详情

To a solution of 2.6 g of 3-oxo-butyric acid methyl ester in THF (50 ml) and 4.6 ml of a solution of sodium methoxide (5.4 M in methanol) was added over 15 minutes a solution of 6.7 g of 2-bromo-1-[2-(trifluoromethoxy)phenyl]-ethanone in 30 ml of THF. The reaction mixture was allowed to stir at room temperature for 17 hours. The solvent was removed, the residue was diluted in diethyl ether and washed several times with water. The organic phase was dried with sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography (silica gel; heptane/ethyl acetate) to give 5.1 g of the title compound. MS (EI) 319.1 (M+H)+.

1. customThe solvent was removed
2. additionthe residue was diluted in diethyl ether
3. washwashed several times with water
4. dry with materialThe organic phase was dried with sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography (silica gel; heptane/ethyl acetate)