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

HRID 1392124

反応式

HRID 1392124 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-3cbb9601a1ed43258aaa8f322aa5f853
出典データセット
uspto-grants-2008_03
特許番号
US07342019B2

関連ノート

読み込み中…