反应详情

温度

20 °C

To a stirred solution of dimethoxymethane (66 mL, 745 mmol) and zinc bromide (0.5 g) in DCM (580 mL) was added drop wise acetyl chloride (53 mL, 745 mmol) during half an hour maintaining the temperature under 20° C. After stirring 3 hours at room temperature, the solution was diluted with DCM (1200 mL), then cooled at 5° C. before the portion wise addition of 1-(2,4,6-trihydroxyphenyl)ethanone (phloroacetophenone) (50 g, 208 mmol) followed by the drop wise addition of DIPEA (208 mL, 1.19 mol). The resulting cloudy solution was stirred overnight, and then was washed with a NH4Cl saturated solution followed by washing with 10% citric acid solution. After drying over Na2SO4, the solvent was removed and the residue (78 g) nearly pure was used for the next step.

1. stirringThe resulting cloudy solution was stirred overnight
2. washwas washed with a NH4Cl saturated solution
3. washby washing with 10% citric acid solution
4. dry with materialAfter drying over Na2SO4
5. customthe solvent was removed