反应详情

A mixture of 1.25 g of 1-[2-hydroxy-4-(4-chlorophenyl)-n-butyl]imidazole and 0.26 g of sodium hydride (50% dispersion in mineral oil) in 20 ml of tetrahydrofuran was stirred under nitrogen at room temperature for one hour, and at 60° C. for one hour. The mixture was then cooled to 0° C. and treated dropwise with stirring with 4-acetylaminobenzyl chloride in 10 ml tetrahydrofuran, keeping the temperature below 10° C. After stirring for one hour, the mixture was heated to 60° C. for 2 hours and poured into water. The product was extracted with ethyl acetate and the extracts dried (MgSO4) and evaporated. The residue was chromatographed on silica gel eluting with 2% water in ethyl acetate to give 1-[4-(4-chlorophenyl)-2-(4-acetylaminobenzyloxy)-n-butyl]imidazole.

1. waitat 60° C. for one hour
2. temperatureThe mixture was then cooled to 0° C.
3. additiontreated dropwise
4. customthe temperature below 10° C
5. stirringAfter stirring for one hour
6. temperaturethe mixture was heated to 60° C. for 2 hours
7. extractionThe product was extracted with ethyl acetate
8. dry with materialthe extracts dried (MgSO4)
9. customevaporated
10. customThe residue was chromatographed on silica gel eluting with 2% water in ethyl acetate