反应详情

温度

25 °C

To a mixture of 104 g of commercially available sodium 2-chloro-5-nitrobenzenesulfonate, 200 ml of acetonitrile and 200 ml of sulfolane stirred at 25° C., was added 153 ml of phosphorus oxychloride over a period of 30 minutes. The temperature was not allowed to exceed 40° C. After completion of the addition, the reaction mixture was heated to 70° C. for 1.5 hours. On cooling to 0° C., the reaction mixture was poured over ice. The resulting solid product was washed with cold water, filtered and air-dried to give 77.6 g of the title compound with a melting point of 87°-89° C.

1. customto exceed 40° C
2. additionAfter completion of the addition
3. temperaturethe reaction mixture was heated to 70° C. for 1.5 hours
4. temperatureOn cooling to 0° C.
5. additionthe reaction mixture was poured over ice
6. washThe resulting solid product was washed with cold water
7. filtrationfiltered
8. customair-dried