Dimethylformamide → 1-[6-(Chloromethyl)pyridin-2-yl]ethanone

HRID 1491824

반응식

HRID 1491824 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

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 24813Phosphorus oxychlorideHCID 103294471-(6-(Hydroxymethyl)pyridin-2-yl)ethanone

생성물 1

HCID 118194451-[6-(Chloromethyl)pyridin-2-yl]ethanone

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

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

  1. temperaturecooling
  2. stirringthe mixture was stirred at the same temperature for 3 hours
  3. washThe separated organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-0de2f0f202d644ee8ae9a1df807c4bcb
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371097

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