反应详情

A solution of p-nitroaniline (1 kg, 7.245 mol) in pyridine (3.6 L) was brought to 45° C. Benzenesulfonyl chloride (1.41 kg, 8 mol) was poured in over 70 minutes, while maintaining the temperature ranging from 45 to 50° C. After 1 hour at 50° C., the reaction medium was poured onto 8 kg of ice and 4.35 L of hydrochloric acid. A yellow precipitate formed and was filtered off by suction and then dissolved in 20 L of 0.5 N sodium hydroxide at 55° C. The insoluble matter was removed by filtration and the filtrate was then neutralized hydrochloric acid while still hot. A yellow precipitate formed and was filtered off by suction, reslurried in water, and then air-dried. 2 kg of product with a melting point of 137° C. were obtained.

1. customwas brought to 45° C
2. temperaturewhile maintaining the temperature
3. customranging from 45 to 50° C
4. customA yellow precipitate formed
5. filtrationwas filtered off by suction
6. dissolutiondissolved in 20 L of 0.5 N sodium hydroxide at 55° C
7. customThe insoluble matter was removed by filtration
8. customA yellow precipitate formed
9. filtrationwas filtered off by suction
10. customair-dried