Pentachlorophenol → alpha-Cyano-phenylacetic acid pentachlorophenylester

HRID 1980227

반응식

HRID 1980227 반응식
[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]

참가 물질

5

반응물 3

HCID 992PentachlorophenolHCID 10868DicyclohexylcarbodiimideHCID 26403alpha-Cyanobenzeneacetic acid

생성물 1

HCID 20402417alpha-Cyano-phenylacetic acid pentachlorophenylester

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-697caea644814226b08ef5af17886796
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04508658

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