Water → 2-(2,4-Dichlorophenyl)-1-(3-pyridyl)-1-propanone

HRID 580502ノート

反応式

HRID 580502 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[Cl:17])=[O:8])[CH:2]=1.[H-].[Na+].[CH3:20]I.O>CN(C)C=O>[Cl:17][C:11]1[CH:12]=[C:13]([Cl:16])[CH:14]=[CH:15][C:10]=1[CH:9]([CH3:20])[C:7]([C:3]1[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=1)=[O:8]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 136712392,4-Dichlorobenzyl 3-pyridyl ketone

生成物 1

HCID 140744312-(2,4-Dichlorophenyl)-1-(3-pyridyl)-1-propanone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

28 g of 2,4-dichlorobenzyl 3-pyridyl ketone are dissolved in 800 ml of dimethylformamide and treated portionwise at 0° C. with 5.5 g of sodium hydride (50% dispersion in oil). After 2 hours at room temperature 14.9 g of methyl iodide are added and the mixture is stirred at room temperature for a further 3 hours. The mixture is then poured into water and extracted with diethyl ether. The organic phase is washed, dried over anhydrous sodium sulfate and subsequently concentrated. By chromatography on silica gel with n-hexane/ethyl acetate (1:2) there is obtained 2-(2,4-dichlorophenyl)-1-(3-pyridyl)-1-propanone as an oil.

後処理

  1. extractionextracted with diethyl ether
  2. washThe organic phase is washed
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationsubsequently concentrated

出典と根拠

ORDレコード
ord-0a4b726cdd534cdf9af701c71168eea2
出典データセット
uspto-grants-1988_06
特許番号
US04753947

反応ノート

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