反应详情

温度

60 °C

A mixture of di(4-chlorophenyl)dimethoxymethane (26 g) (see Preparation 13) and methyl (3,4-dihydroxyphenyl)acetate (16 g) (see Preparation 12) in toluene (200 ml) was heated under reflux in a Dean-Stark apparatus for one hour. The reaction was cooled to 60° C. and p-toluenesulphonic acid was added (50 mg). After heating under reflux for 16 hours the solution was cooled, washed with aqueous sodium bicarbonate (100 ml), dried (MgSO4) and evaporated to a brown gum. Flash chromatography (silica, eluant=4:1 hexane/ethyl acetate) gave the title compound as a pale yellow gum (13.7 g). LRMS m/z=415(m)+.

1. temperaturewas heated
2. temperatureunder reflux in a Dean-Stark apparatus for one hour
3. temperatureAfter heating
4. temperatureunder reflux for 16 hours the solution
5. temperaturewas cooled
6. washwashed with aqueous sodium bicarbonate (100 ml)
7. dry with materialdried (MgSO4)
8. customevaporated to a brown gum