反应详情

温度

20 °C

In a 1-liter four-necked glass flask is prepared a solution mixture of 100 g of 4-chloro-3-ethylphenol and 350 g of dichloroethane. While the mixture is maintained at a temperature of 35°-45° C., 80 g of chlorosulfonic acid is added dropwise and the mixture is maintained at a temperature of 40°-45° C. for 1 hour. Next, 326 g of a 14.3% hydrochloric acid solution is added, and 68 g of a 35% aqueous hydrogen peroxide solution is added dropwise while maintaining the temperature at 40°-45° C. After the mixture is maintained at the same temperature for 8 hours, it is cooled to 20° C. After the oily layer is separated, the aqueous layer obtained is charged in a 1-liter four-necked glass flask, and 172 g of a 70% nitric acid solution is added dropwise to the aqueous a temperature of 30°-40° C. The liquid becomes turbid and turns yellowish white. The temperature is raised about 15° C. After the addition, the reaction mixture is maintained at the same temperature for 1 hour. The reaction mixture is cooled to 5° C. and filtered. The product is washed with water and dried to give 2,4-dichloro-3-ethyl-6-nitrophenol.

1. customIn a 1-liter four-necked glass flask is prepared
2. additionis added dropwise
3. temperaturethe mixture is maintained at a temperature of 40°-45° C. for 1 hour
4. temperaturewhile maintaining the temperature at 40°-45° C
5. temperatureAfter the mixture is maintained at the same temperature for 8 hours
6. customAfter the oily layer is separated
7. customthe aqueous layer obtained
8. additionis charged in a 1-liter four-necked glass flask
9. temperatureThe temperature is raised about 15° C
10. additionAfter the addition
11. temperaturethe reaction mixture is maintained at the same temperature for 1 hour
12. temperatureThe reaction mixture is cooled to 5° C.
13. filtrationfiltered
14. washThe product is washed with water
15. customdried