반응 #427666

반응 방정식

methyl iodide

chloroform

5-nitro-3-(2H-1,2,3-triazol-2-yl)pyridin-2-ol

5-nitro-3-(1H-1,2,3-triazol-1-yl)pyridin-2-ol

→

1-methyl-5-nitro-3-(2H-1,2,3-triazol-2-yl)pyridin-2(1H)-one

1-methyl-5-nitro-3-(1H-1,2,3-triazol-1-yl)pyridin-2(1H)-one

용매

Water

반응 조건

후처리

1. 1
   workup.ADDITIONcontaining
2. 2
   기타obtained in the 1st step
3. 3
   온도by reflux for 2 hours
4. 4
   추출followed by extraction with ethyl acetate
5. 5
   세척The resultant was washed with saturated saline
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONSubsequently, the solvent was distilled away under reduced pressure
8. 8
   기타the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=2:5 to 2:3)

실험 절차

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.

출처