反应详情

A mixture of 1,5-dimethyl-2-(4-trifluoromethylphenyl)imidazole (0.6 g), aqueous formaldehyde (3.5 ml of 36%), sodium acetate (0.6 g), and acetic acid (0.5 ml) was refluxed for 24 hours. The mixture was cooled, and concentrated sodium hydroxide added until the mixture was just: basic, keeping the temperature at about 10° C. The mixture was extracted with methylene chloride, and solvent removed from the organic layer under reduced pressure. The residue was flash-chromatographed on silica gel, eluting with methylene chloride containing methanol (97/3), to yield 0.4 g of 1,5-dimethyl-4-hydroxymethyl-2-(4-trifluoromethyl-phenyl)imidazole, m.p. 152° C.

1. temperaturewas refluxed for 24 hours
2. temperatureThe mixture was cooled
3. customat about 10° C
4. extractionThe mixture was extracted with methylene chloride, and solvent
5. customremoved from the organic layer under reduced pressure
6. customThe residue was flash-chromatographed on silica gel
7. washeluting with methylene chloride
8. additioncontaining methanol (97/3)