Dimethylformamide → 1-[6-(Chloromethyl)pyridin-2-yl]ethanone
반응식
P(Cl)(Cl)([Cl:3])=O.[C:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15]O)[N:10]=1)(=[O:8])[CH3:7].CN(C)C=O.C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.O>[C:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][Cl:3])[N:10]=1)(=[O:8])[CH3:7]참가 물질
7
실험 절차
Phosphorus oxychloride (7.8 ml) was dropwise added to a mixture of 2-acetyl-6-hydroxymethylpyridine (10.0 g) and N,N-dimethylformamide (15.4 ml) in ethyl acetate (100 ml) under ice-cooling with stirring and the mixture was stirred at the same temperature for 3 hours. The reaction mixture was added to water and adjusted to pH 7.5 with potassium carbonate. The separated organic layer was washed with brine, dried over magnesium sulfate and evaporated to give 2-acetyl-6-chloromethylpyridine (10.85 g) as an oil.
후처리
- temperaturecooling
- stirringthe mixture was stirred at the same temperature for 3 hours
- washThe separated organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- customevaporated
출처 및 근거
- ORD 기록
- ord-b49227bd87f64e7ba28744faa948c3c7
- 출처 데이터셋
- uspto-grants-1994_11
- 특허 번호
- US05364871
반응 노트
불러오는 중…