反应详情

To a suspension of 21 g of α-(2,6-dimethyl-4-carboxyphenyl)-2-chloro-5-iodobenzenemethanol, 5.1 g of imidazole, 13.8 g of potassium carbonate and 120 ml of dimethylformamide are added 0.4 g of potassium fluoride and 0.4 g of copper powder, and the mixture is stirred at 135°-140° C. for 30 hours. After cooling, to the reaction mixture is added 240 ml of water and 0.45 g of sodium sulfide trihydrate. The whole mixture is stirred for 30 minutes. The precipitated copper sulfide is filtered with sellaite under reduced pressure and the filtrate is adjusted to pH 4 with concentrated hydrochloric acid under heating and stirring. The precipitated crystals are collected by filtration, washed with water and then dried. Recrystallization from dimethylformamide gives α-(2,6-dimethyl-4-carboxyphenyl)-2-chloro-5-(1-imidazolyl)benzenemethanol, melting at 318°-320° C. with decomposition, as white crystals in high yield.

1. temperatureAfter cooling, to the reaction mixture
2. stirringThe whole mixture is stirred for 30 minutes
3. filtrationThe precipitated copper sulfide is filtered with sellaite under reduced pressure
4. temperatureunder heating
5. stirringstirring
6. filtrationThe precipitated crystals are collected by filtration
7. washwashed with water
8. customdried
9. customRecrystallization from dimethylformamide