Phenol → 2-(Ethylthio)phenol

HRID 745691

Reaktionsgleichung

Reaktionsgleichung von HRID 745691
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:8]([S:10]SCC)[CH3:9]>[O-]C1C=CC=CC=1.[Zr+4].[O-]C1C=CC=CC=1.[O-]C1C=CC=CC=1.[O-]C1C=CC=CC=1>[CH2:8]([S:10][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[OH:7])[CH3:9]

Komponenten

4

Edukt 2

HCID 996PhenolHCID 8077Diethyl disulfide

Produkt 1

HCID 1224072-(Ethylthio)phenolAusbeute 38 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13847644Zirconium(2+);tetraphenoxideKatalysator

Reaktionsbedingungen

Temperatur
195 °C

Versuchsvorschrift

Zirconium phenoxide (4.0 g, 0.0086 moles) was added to phenol (8.9 g, 0.095 moles) and ethyl disulfide (10.5 g, 0.086 moles). The mixture was heated under nitrogen for 6.5 hours during which the temperature slowly increased to 195° C. Ethyl mercaptan was removed continuously by distillation. The mixture was distilled at 0.4 mm mercury to a maximum head temperature of 102° C. yielding 12.2 g of distillate. Gas chromatographic (GC) analysis indicated the distillate contained 5.0 g of ortho-(ethylthio)phenol (38% yield).

Aufarbeitung

  1. temperatureThe mixture was heated under nitrogen for 6.5 hours during which the temperature
  2. customEthyl mercaptan was removed continuously by distillation
  3. distillationThe mixture was distilled at 0.4 mm mercury to a maximum head temperature of 102° C.
  4. customyielding 12.2 g of distillate

Quellen und Nachweise

ORD-Eintrag
ord-d5c6c32db05f45e4a3c4fbb957a38a0f
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04599451

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