Phenol → 2-(Ethylthio)phenol

HRID 745691

반응식

HRID 745691 반응식
[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]

참가 물질

4

반응물 2

HCID 996PhenolHCID 8077Diethyl disulfide

생성물 1

HCID 1224072-(Ethylthio)phenol수율 38%

시약·촉매·용매 1

HCID 13847644Zirconium(2+);tetraphenoxide촉매

반응 조건

온도
195 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d5c6c32db05f45e4a3c4fbb957a38a0f
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599451

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