反应详情

温度

120 °C

A mixture of 2,4-dichloro-bromobenzene (22.6 g), N-[(±)-2-(4-hydroxyphenoxy)propionyl]isoxazolidine (23.7 g) which was prepared as in Example 3, anhydrous potassium carbonate (14.5 g) and dimethylsulfoxide (200 ml) was stirred at 120° C. for 4 hours. After the reaction mixture was cooled, water and benzene were added thereto whereby to form two layers. The organic layer so separated was washed with 1 N aqueous sodium hydroxide solution and then with water and dried over anhydrous sodium sulfate. Removal of the solvent by a distillation in vacuo gave N-[(±)-2-[4-(2,4-dichlorophenoxy)phenoxy]propionyl]isoxazolidine (30.9 g) as a pale yellow crystalline solid. Recrystallization from a mixture of n-hexane/ethyl acetate yielded a white crystalline solid. m.p. 115°-118° C.

1. temperatureAfter the reaction mixture was cooled
2. customwhereby to form two layers
3. customThe organic layer so separated
4. washwas washed with 1 N aqueous sodium hydroxide solution
5. dry with materialwith water and dried over anhydrous sodium sulfate
6. customRemoval of the solvent
7. distillationby a distillation in vacuo