Pentachlorophenol → alpha-Cyano-phenylacetic acid pentachlorophenylester

HRID 1980227

Reaktionsgleichung

Reaktionsgleichung von HRID 1980227
[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]

Komponenten

5

Edukt 3

HCID 992PentachlorophenolHCID 10868DicyclohexylcarbodiimideHCID 26403alpha-Cyanobenzeneacetic acid

Produkt 1

HCID 20402417alpha-Cyano-phenylacetic acid pentachlorophenylester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-697caea644814226b08ef5af17886796
Quelldatensatz
uspto-grants-1985_04
Patentnummer
US04508658

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