反应详情

温度

25 °C

A mixture of o-chlorobenzoic acid (2.0 kg.) and chlorosulfonic acid (10.5 kg.) is heated at 90°-100° C. for 5 hours. The reaction mixture is cooled to 25° C. and then slowly poured into a 10 liter mixture of ice and water. The addition requires about 1 hour, and the temperature is maintained below 10° C. during this period by the addition of more ice. The final volume of slurry after the quench is about 40 liters. The solid material is collected and thoroughly washed on the funnel with fresh water. The crude wet cake is dissolved in 16 liters of diethyl ether. The ether layer is washed once with 2 liters of saturated aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The filtered ether solution is concentrated in vacuo with the continual addition of hexane. The resulting hexane slurry is concentrated to a final volume of approximately 8 liters and filtered. The crystalline cake is washed with hexane and dried in the atmosphere to give 2.5 kg. of product (76.8% of theory), m.p. 149°-151° C.

1. temperatureis heated at 90°-100° C. for 5 hours
2. additionThe addition
3. temperaturethe temperature is maintained below 10° C. during this period by the addition of more ice
4. customThe solid material is collected
5. washthoroughly washed on the funnel with fresh water
6. dissolutionThe crude wet cake is dissolved in 16 liters of diethyl ether
7. washThe ether layer is washed once with 2 liters of saturated aqueous sodium chloride solution
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationThe filtered ether solution is concentrated in vacuo with the continual addition of hexane
10. concentrationThe resulting hexane slurry is concentrated to a final volume of approximately 8 liters
11. filtrationfiltered
12. washThe crystalline cake is washed with hexane
13. customdried in the atmosphere
14. customto give 2.5 kg