Potassium Cyanide → 2-(3,5-Dichlorophenyl)acetonitrile

HRID 232607

反応式

HRID 232607 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:10])[CH:9]=1)[CH2:5]Cl.[C-:11]#[N:12].[K+]>ClCCl.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:5][C:11]#[N:12])[CH:7]=[C:8]([Cl:10])[CH:9]=1

参加物

6

反応物 2

HCID 9032Potassium CyanideHCID 1378803,5-Dichlorobenzyl chloride

生成物 1

HCID 126899782-(3,5-Dichlorophenyl)acetonitrile

試薬・触媒・溶媒 3

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a vigorously stirred solution of 3,5-dichlorobenzylchloride (28 g) in dichloromethane (150 ml) was added a mixture of KCN (27.5 g) and tetrabutylammonium hydrogen sulphate (2.38 g) in water (110 ml). After stirring at room temperature for 22 hours, the mixture was diluted with dichloromethane, the organic phase washed with water and concentrated in vacuo to leave an oil. Filtration through silica with toluene followed by concentration then trituration with hexane gave the desired product as a colourless solid. 15.8 g, mp. 31°-32° C.

後処理

  1. washthe organic phase washed with water
  2. concentrationconcentrated in vacuo
  3. customto leave an oil
  4. filtrationFiltration through silica with toluene
  5. concentrationfollowed by concentration

出典と根拠

ORDレコード
ord-b467563f072e4b279b42eeb189668640
出典データセット
uspto-grants-1997_01
特許番号
US05591746

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