反应详情

Silver carbonate (377 mg) and methyl iodide (366 W) were added to a chloroform (10 ml) solution containing the mixture of 5-nitro-3-(2H-1,2,3-triazol-2-yl)pyridin-2-ol and 5-nitro-3-(1H-1,2,3-triazol-1-yl)pyridin-2-ol (184 mg) obtained in the 1st step while shielding light, followed by reflux for 2 hours. Water was added, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=2:5 to 2:3), and a white solid of 1-methyl-5-nitro-3-(2H-1,2,3-triazol-2-yl)pyridin-2(1H)-one (28.1 mg) and a white solid of 1-methyl-5-nitro-3-(1H-1,2,3-triazol-1-yl)pyridin-2(1H)-one (23.3 mg) were thus obtained.

1. additioncontaining
2. customobtained in the 1st step
3. temperatureby reflux for 2 hours
4. extractionfollowed by extraction with ethyl acetate
5. washThe resultant was washed with saturated saline
6. dry with materialdried over anhydrous sodium sulfate
7. distillationSubsequently, the solvent was distilled away under reduced pressure
8. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=2:5 to 2:3)