Hydrochloric Acid → 2-Chloro-1-(2,4-dihydroxyphenyl)ethan-1-one

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence