反应详情

温度

80 °C

N,N-dimethylformamide di-tert-butyl acetal (75 ml, 0.31 mol) in toluene (60 ml) was added dropwise over 1.5 hours to 2,6-difluoro-4-methoxy-benzoic acid (15 g, 80 mmol)(Mol. Cryst. Liq. Cryst. 1989, 172) in toluene (120 ml) at 80° C. under a nitrogen atmosphere. The mixture was stirred at 80° C. for 30 minutes and then cooled to room temperature. Ethyl acetate (100 ml) was added and the organic solution was washed with saturated sodium hydrogen carbonate solution (2×150 ml), brine (150 ml), dried over magnesium sulphate and evaporated under reduced pressure. The residue was purified by chromatography on silica gel using diethyl ether in pentane as eluant (10:90) to give the title compound as an oil (17.91 g).

1. temperaturecooled to room temperature
2. washthe organic solution was washed with saturated sodium hydrogen carbonate solution (2×150 ml), brine (150 ml)
3. dry with materialdried over magnesium sulphate
4. customevaporated under reduced pressure
5. customThe residue was purified by chromatography on silica gel