反应详情

The title compound was obtained using the following procedure: The sulfamoyl chloride solution prepared in (a) was reacted as in Example 4 with 17.3 g (0.100 mole) of 2-(2-chlorophenoxy)ethanol and 40.4 g (0.400 mole) of triethylamine in 100 ml of acetonitrile followed by extraction, washing and concentration procedures of Example 4 through the first evaporation. The viscous, oily residue was partitioned between 500 ml of water and 500 ml of ethyl ether. The organic layer was washed with four 300 ml portions of water (pH of wash finally neutral to pH paper), dried over magnesium sulfate and the solvent evaporated under reduced pressure to give a white solid. The solid was recrystallized from ethyl ether-petroleum ether (bp 30°-60° C.) to give 14.5 g (58%) of title compound as white solid, mp 84.5°-86° C.

1. extractionfollowed by extraction
2. washwashing
3. concentrationconcentration procedures of Example 4
4. customthrough the first evaporation
5. customThe viscous, oily residue was partitioned between 500 ml of water and 500 ml of ethyl ether
6. washThe organic layer was washed with four 300 ml portions of water (pH
7. washof wash finally neutral to pH paper),
8. dry with materialdried over magnesium sulfate
9. customthe solvent evaporated under reduced pressure
10. customto give a white solid
11. customThe solid was recrystallized from ethyl ether-petroleum ether (bp 30°-60° C.)