反应详情

The ethanol solution of the product of step B, above, (about 10 m moles) was added to a solution of 0.46 sodium (0.02 g-atoms) in 10 ml ethanol at 4° C. under nitrogen. After 5 minutes, a solution of 1.67 g (10 m moles) of 4-methyl-5-chloromethylimidazole.HCl in 14 ml ethanol was added and the mixture was stirred at room temperature under nitrogen for 70 minutes. The reaction mixture was filtered through a bed of celite filter aid to remove the inorganic salts and the celite was washed with ethanol. The filtrate was evaporated to dryness and the product was purified by chromatography on a silica gel column (20 g silica, 3.2×4.5 cm bed) with ethanol-chloroform mixtures as the solvent. The ethanol content was gradually increased from 2 to 15%. The eluant was evaporated to dryness to give 1.906 g of crystalline product. Recrystallization from 2-propanol gave 1.49 g (54%) of the title product, m.p. 144°-145° C.

1. filtrationThe reaction mixture was filtered through a bed of celite filter aid
2. customto remove the inorganic salts
3. washthe celite was washed with ethanol
4. customThe filtrate was evaporated to dryness
5. customthe product was purified by chromatography on a silica gel column (20 g silica, 3.2×4.5 cm bed) with ethanol-chloroform mixtures as the solvent
6. temperatureThe ethanol content was gradually increased from 2 to 15%
7. customThe eluant was evaporated to dryness