Phenol → 2-(Ethylthio)phenol

HRID 745691

反応式

HRID 745691 の反応式
[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]

参加物

4

反応物 2

HCID 996PhenolHCID 8077Diethyl disulfide

生成物 1

HCID 1224072-(Ethylthio)phenol収率 38%

試薬・触媒・溶媒 1

HCID 13847644Zirconium(2+);tetraphenoxide触媒

反応条件

温度
195 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d5c6c32db05f45e4a3c4fbb957a38a0f
出典データセット
uspto-grants-1986_07
特許番号
US04599451

関連ノート

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