Chlorodifluoromethane → HCID 14796596, compound

Participants

Reaction Steps

In a 100 ml autoclave, 5.87 g (0.03 mol) 3-(4-chlorophenyl)-5-(4H)-isoxazolone was dissolved 30 ml dioxane and treated with 10 ml of 30% aqueous potassium hydroxide. The autoclave was pressurised to 10 bar with chlorodifluoromethane and the reaction mixture was heated at 50°-60° C. for 15 hours. After cooling and reducing the pressure the solution was poured into 300 ml ice/water and extracted three times with 70 ml ethyl acetate. The combined organic phases were dried over magnesium sulphate and concentrated. The residue was purified by column chromatography.

Provenance & Evidence