Methyl iodide → 2,5-Dichloro-4-methoxypyridine
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([OH:8])[C:5]([Cl:9])=[CH:4][N:3]=1.[C:10]([O-])([O-])=O.[K+].[K+].CI>CN(C=O)C.CC(=O)OCC>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:10])[C:5]([Cl:9])=[CH:4][N:3]=1参加物
6
実験手順
To a solution of 2,5-dichloro-4-hydroxypyridine (1.43 g, 8.73 mmol) in DMF (15 mL), K2CO3 (2.41 g, 17.5 mmol) followed by methyl iodide (1.48 g, 8.73 mmol) is added. The mixture is stirred at rt for 24 h before it is diluted with EA (200 mL), washed with water (2×100 mL), dried over MgSO4, filtered and concentrated. The crude product is purified by CC on silica gel eluting with heptane:EA 1:1 to give 2,5-dichloro-4-methoxy-pyridine (0.73 g) as a white solid; LC-MS: tR=0.85 min; [M+1]+=177.90.
後処理
- additionis added
- washwashed with water (2×100 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude product is purified by CC on silica gel eluting with heptane:EA 1:1
出典と根拠
- ORDレコード
- ord-344f1705119e43c1814c8609c679a8d6
- 出典データセット
- uspto-grants-2013_12
- 特許番号
- US08598208B2
反応ノート
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