Pentachlorophenol → alpha-Cyano-phenylacetic acid pentachlorophenylester

HRID 1980227

反応式

HRID 1980227 の反応式
[C:1]([CH:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:4]([OH:6])=[O:5])#[N:2].C1(N=C=NC2CCCCC2)CCCCC1.[Cl:28][C:29]1[C:34](O)=[C:33]([Cl:36])[C:32]([Cl:37])=[C:31]([Cl:38])[C:30]=1[Cl:39]>ClCCl>[Cl:28][C:29]1[C:34]([O:5][C:4](=[O:6])[CH:3]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:1]#[N:2])=[C:33]([Cl:36])[C:32]([Cl:37])=[C:31]([Cl:38])[C:30]=1[Cl:39]

参加物

5

反応物 3

HCID 992PentachlorophenolHCID 10868DicyclohexylcarbodiimideHCID 26403alpha-Cyanobenzeneacetic acid

生成物 1

HCID 20402417alpha-Cyano-phenylacetic acid pentachlorophenylester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

8 g. (0.05 moles) of α-cyano-phenylacetic acid are dissolved in 80 ml. of dichloromethane. 10.3 g. (0.05 moles) of dicyclohexylcarbodiimide and 13 g. (0.05 moles) of pentachlorophenol are added dropwise dissolved in 50 ml. of dichloromethane. The mixture is stirred for 4 hours, cooled to 0° C. and the precipitated dicyclohexylurea is filtered. The filtered substance is washed twice on the filter with 15 ml. of dichloromethane. The combined organic layers are distilled off and the precipitated ester is taken up with 20 ml. of diisopropyl ether and the crystals are filtered, washed twice with diisopropyl ether and dried.

後処理

  1. dissolutiondissolved in 50 ml
  2. filtrationthe precipitated dicyclohexylurea is filtered
  3. washThe filtered substance is washed twice on the
  4. filtrationfilter with 15 ml
  5. distillationThe combined organic layers are distilled off
  6. filtrationof diisopropyl ether and the crystals are filtered
  7. washwashed twice with diisopropyl ether
  8. customdried

出典と根拠

ORDレコード
ord-697caea644814226b08ef5af17886796
出典データセット
uspto-grants-1985_04
特許番号
US04508658

関連ノート

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