反应详情

A solution of 12 g (0.031 mol) of α-(2,4-dichlorophenyl)-α-(p-fluorophenyl)-1-(methoxymethyl)imidazole-2-methanol, 150 ml. of glacial acetic acid, 15 ml. of concentrated hydrochloric acid and 15 ml. of water was refluxed for 5 hours. The dark brown solution was concentrated and water was added to the residue. The mixture was then made alkaline by addition of ammonia and extracted with diethyl ether. The organic phase was separated off, decolorized with active charcoal, dried over sodium sulphate and the ether was distilled off. The solid residue was twice crystallised from acetone, rewashed with petroleum ether (boiling range 60°-80° C.) and once crystallised from isopropyl alcohol. α-(2,4-Dichlorophenyl)-α-(p-fluorophenyl)imidazole-2-methanol was obtained. Melting point 193.5°-194° C.

1. concentrationThe dark brown solution was concentrated
2. additionwater was added to the residue
3. additionby addition of ammonia
4. extractionextracted with diethyl ether
5. customThe organic phase was separated off
6. dry with materialdried over sodium sulphate
7. distillationthe ether was distilled off
8. customThe solid residue was twice crystallised from acetone
9. customonce crystallised from isopropyl alcohol