反应详情

温度

24 °C

Molten 2,4-dichlorophenol (164.27 g) was added to 332 ml of chlorosulfonic acid at 36°-40° C. over one and one-half hours. After a 10 minute hold period at 38°-40° C. the reaction mixture was cooled to 24° C. and held for 1 hour. This solution was then pumped into 500 ml of water which had been cooled to 5° C. External cooling was required to maintain the quench slurry at 60° C. Once the quench was complete, the slurry was cooled to 45° C. and the agitation was stopped to allow the solids to settle. Using a dipstick, 380 ml of supernatent was removed. This volume was replaced with 180 ml H2O and 200 ml CH2Cl2. The organic layer was separated and a second 50 ml wash with CH2Cl2 was obtained and combined with the first to provide 340 ml, 489 g of a 40.3% solution of (C) in CH2Cl2 (81% yield).

1. waitheld for 1 hour
2. temperaturehad been cooled to 5° C
3. temperatureExternal cooling
4. temperatureto maintain the quench slurry at 60° C
5. temperaturethe slurry was cooled to 45° C.
6. customwas removed
7. customThe organic layer was separated
8. washa second 50 ml wash with CH2Cl2
9. customwas obtained