反应详情

To a solution of 4-chloromethyl-5-methyl-2-phenyl-1H-imidazole hydrochloride (4.86 g) [CAS 58731-95-6] in DMF (50 ml) was added sodium azide (7.79 g). The reaction mixture was stirred at room temperature for 18 h under argon and concentrated without heating under high vacuum. To the residue was added ice/1 molar K2CO3 solution, and the mixture was extracted with ethyl acetate. The organic phase was washed with brine, dried over magnesium sulphate and concentrated. The residue was purified by chromatography on silica gel using methylene chloride/methanol 2% as eluent to obtain 4-azidomethyl-5-methyl-2-phenyl-1H-imidazole (3.70 g) as a light yellow amorphous powder.

1. concentrationconcentrated
2. temperaturewithout heating under high vacuum
3. additionTo the residue was added ice/1 molar K2CO3 solution
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organic phase was washed with brine
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated
8. customThe residue was purified by chromatography on silica gel