反应详情

An 85.38 g. (0.25 mole) portion of 2,3-dichloro-4-(4'-hydroxybenzoyl)phenoxyacetic acid, 34.5 g. (0.75 mole) of ethanol, and 100 ml. of ethylene dichloride, using 3.5 ml. of sulfuric acid as the catalyst was mixed and refluxed with stirring overnight according to the procedure of Clinton and Laskowski, J.A.C.S. 70 3135, 1948. The acid gradually went into solution. The reaction layer was cooled, separated and the organic layer washed successively with water, twice with KHCO3 solution and finally with water. The dried ethylene dichloride was evaporated to dryness to give an oil which solidified to give 86 g. crude ester on trituration with pentane and filtering; m.p. 127°-9° (93% yield). This material was used without further purification in subsequent experiments.

1. temperaturerefluxed
2. temperatureThe reaction layer was cooled
3. customseparated
4. washthe organic layer washed successively with water, twice with KHCO3 solution and finally with water
5. customThe dried ethylene dichloride was evaporated to dryness
6. customto give an oil which
7. customto give 86 g
8. filtrationcrude ester on trituration with pentane and filtering
9. customThis material was used without further purification in subsequent experiments