反应详情

To a solution of 80 g of 2-chloro-5nitrobenzenesulfonyl chloride (Example A-1 above) in 200 ml of methylene chloride heated to reflux, was slowly added a solution of 30 g of dimethylamine hydrochloride in 30 ml of water followed by a dropwise addition of triethylamine. After completion of the addition, the reaction mixture was refluxed for 20 minutes, cooled to room temperature and concentrated by rotatory evaporation. The residue was treated with water and the resulting solid was filtered and recrystallized from ethanol, affording 61 g of the title compound, mp 138°-140° C.

1. temperatureto reflux
2. additionAfter completion of the addition
3. temperaturethe reaction mixture was refluxed for 20 minutes
4. concentrationconcentrated by rotatory evaporation
5. additionThe residue was treated with water
6. filtrationthe resulting solid was filtered
7. customrecrystallized from ethanol