Pyridine → 1-(4-Chlorophenyl)-2-(2,4-dichlorophenyl)ethane-1,2-dione

HRID 1452508

反応式

HRID 1452508 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[Cl:18])=[O:10])=[CH:4][CH:3]=1.C1C=C[NH+]=CC=1.[O-:25][Cr](Cl)(=O)=O.N1C=CC=CC=1>ClCCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:25])[C:9]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[Cl:18])=[O:10])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 219848672-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)ethan-1-oneHCID 178418287HCID 178418287、化合物

生成物 1

HCID 220660771-(4-Chlorophenyl)-2-(2,4-dichlorophenyl)ethane-1,2-dione

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
25 °C

実験手順

2-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)ethanone (2.7 g, 9.01 mmol) was dissolved in 1,2-dichloroethane (25 ml) and freshly made PCC (3.89 g, 18.02 mmol), pyridine (1.43 g, 18.02 mmol) and molecular sieves were added. The reaction mixture was refluxed under inert atmosphere overnight. The solution was cooled to 25° C., filtered through Silica and then solvent was evaporated under reduced pressure. The crude product (1.9 g, 66%) was used directly in the next step. 1H NMR (500 MHz) δ 7.97 (d, 2H), 7.84 (d, 1H), 7.52 (d, 2H), 7.46 (s, 1H), 7.44 (d, 1H).

後処理

  1. temperatureThe reaction mixture was refluxed under inert atmosphere overnight
  2. filtrationfiltered through Silica
  3. customsolvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-51ee4d950a064eb9828639cacff9be8e
出典データセット
uspto-grants-2009_01
特許番号
US07473693B2

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