Methyl iodide → Methyl 3-chloropyrazine-2-carboxylate
反応式
[Cl:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1.[C:11](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C=O)C>[Cl:1][C:2]1[C:3]([C:8]([O:10][CH3:11])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1参加物
5
実験手順
To a suspension of 3-chloropyrazine-2-carboxylic acid (10 g, 63 mmol) and cesium carbonate (31 g, 95 mmol) in DMF was added iodomethane (5.9 ml, 95 mmol). The solution was stirred for 48 hours. After that time, the reaction was removed from stirring, acidified to pH 5 with 1.0 N HCl and extracted five times with ethyl acetate. The combined organics were dried over sodium sulfate, filtered, and concentrated, affording to target material as an orange oil. MS (ESI, pos. ion) m/z: 173.0 (M+1).
後処理
- customAfter that time, the reaction was removed
- stirringfrom stirring
- extractionextracted five times with ethyl acetate
- dry with materialThe combined organics were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customaffording
出典と根拠
- ORDレコード
- ord-a9da39d2f2a24814951eb10364b1bdd1
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637500B2
反応ノート
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