Methyl iodide → 2,5-Dichloro-4-methoxypyridine
반응식
[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]=1참가 물질
6
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-344f1705119e43c1814c8609c679a8d6
- 출처 데이터셋
- uspto-grants-2013_12
- 특허 번호
- US08598208B2
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