Methyl iodide → 4-(4-Methyl-5-(methylthio)-4H-1,2,4-triazol-3-yl)pyridine
반응식
[CH3:1][N:2]1[C:6]([C:7]2[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=2)=[N:5][NH:4][C:3]1=[S:13].I[CH3:15]>[OH-].[Na+].C(O)C>[CH3:1][N:2]1[C:3]([S:13][CH3:15])=[N:4][N:5]=[C:6]1[C:7]1[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=1참가 물질
5
실험 절차
To a solution of 4-Methyl-5-pyridin-4-yl-2,4-dihydro-[1,2,4]triazole-3-thione (1000 mg, 5.20 mmol) in 1M sodium hydroxide (10 mL), added a solution of iodomethane (0.52 mL, 8.32 mmol) in ethanol (3 mL). Stirred at RT overnight. Extracted into 200 mL dichloromethane and washed with brine (50 mL). Dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to yield title compound (1.00 g, 94% yield). 1H-NMR (CDCl3) δ (ppm): 8.81 (d, 2H), 7.62 (d, 2H), 3.68 (s, 3H), 2.82 (s, 3H).
후처리
- extractionExtracted into 200 mL dichloromethane
- washwashed with brine (50 mL)
- dry with materialDried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-6758800d16a04f16869d642e6b765ce4
- 출처 데이터셋
- uspto-grants-2010_04
- 특허 번호
- US07691892B2
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