反应详情

温度

27 °C

A 100L round bottomed flask (RBF) containing 34.0 L of 1,4-dioxane was charged with 5.0 kg of HCl gas through a subsurface line. Resorcinol (10.0 kg) was then added as a solid, followed by addition of solid ZnCl2 (6.20 kg). A slight exotherm from 21 to 29° C. occurred after the ZnCl2 addition. The mixture was cooled with an ice/water bath, and chloroacetonitrile (7.50 kg) was added in portions over 2 h while maintaining the temperature at <40° C. The reaction mixture was aged 9 h at room temperature, and then water (34 L) was charged over 0.5 h. An exotherm to 40° C. occurred at the beginning of the water addition, and the reaction eventually cooled to 27° C. by the end of the addition. The resulting slurry was aged for 11 h at room temperature. More water (14L) was added, and the slurry was cooled to 0° C. The slurry was filtered, washed with water (4×20L), and then dried under a fast flow of nitrogen. After 5 days of drying, the chloroketone 2 was isolated as a light pink solid.

1. customfrom 21 to 29° C.
2. temperatureThe mixture was cooled with an ice/water bath
3. temperaturewhile maintaining the temperature at <40° C
4. customthe reaction
5. waitThe resulting slurry was aged for 11 h at room temperature
6. temperaturethe slurry was cooled to 0° C
7. filtrationThe slurry was filtered
8. washwashed with water (4×20L)
9. customdried under a fast flow of nitrogen
10. customAfter 5 days of drying