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

HRID 2379806

反応式

HRID 2379806 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b49227bd87f64e7ba28744faa948c3c7
出典データセット
uspto-grants-1994_11
特許番号
US05364871

関連ノート

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