Methyl iodide → 4-(4-Methyl-5-(methylthio)-4H-1,2,4-triazol-3-yl)pyridine
反応式
[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]=1参加物
5
実験手順
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).
後処理
- extractionExtracted into 200 mL dichloromethane
- washwashed with brine (50 mL)
- dry with materialDried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-6758800d16a04f16869d642e6b765ce4
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07691892B2
反応ノート
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