反应详情

4.7 g of acetyl chloride are added dropwise at 10°-20° C. to a mixture of 5.55 g of 1-[2-chloro-4-(3-chlorophenoxy)phenoxy]-2-ethylaminocarbonyloxyethane, 3.6 g of pyridine, 0.15 g of dimethylaminopyridine and 60 ml of toluene. The mixture is then stirred for 50 hours at reflux temperature. The batch is poured into 300 ml of ice-water and is extracted three times using diethyl ether. The combined ether phases are washed using 1N hydrochloric acid and three times using water, dried over sodium sulfate and the solvent is evaporated in vacuo. The crude product is purified on silica gel using diethyl ether/n-hexane (2:7) as mobile phase. This gives the title compound of refractive index nD20 1.5640.

1. temperatureat reflux temperature
2. extractionis extracted three times
3. washThe combined ether phases are washed
4. dry with materialdried over sodium sulfate
5. customthe solvent is evaporated in vacuo
6. customThe crude product is purified on silica gel