Water → 2,6-Bis(1,1-dimethylethyl)-4-(methylthio)phenol

HRID 231589

反応式

HRID 231589 の反応式
[CH3:1][C:2]([C:5]1[CH:6]=[C:7]([S:16][C:17]#N)[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])[CH3:3].C(OP(OCC)OCC)C.O>CO>[CH3:4][C:2]([C:5]1[CH:6]=[C:7]([S:16][CH3:17])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:1])[CH3:3]

参加物

5

反応物 3

HCID 962WaterHCID 31215Triethyl phosphiteHCID 6192452,6-DI-Tert-butyl-4-thiocyanato-phenol

生成物 1

HCID 144799522,6-Bis(1,1-dimethylethyl)-4-(methylthio)phenol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 3,5-bis(1,1-dimethylethyl)-4-hydroxyphenylthiocyanate (238 g, 0.90 mole), triethylphosphite (225 g, 1.35 mole), water (200 g), and methanol (2000 ml) was stirred at reflux for two hours. Upon cooling, the mixture was concentrated in vacuo. The residue was triturated with water, and the solid was collected by filtration and air dried. Recrystallization from aqueous methanol gave the title compound, m.p. 69°-71°.

後処理

  1. temperatureat reflux for two hours
  2. temperatureUpon cooling
  3. concentrationthe mixture was concentrated in vacuo
  4. customThe residue was triturated with water
  5. filtrationthe solid was collected by filtration and air
  6. customdried
  7. customRecrystallization from aqueous methanol

出典と根拠

ORDレコード
ord-eb54f59a4b2e411eb36221891cf989dc
出典データセット
uspto-grants-1989_07
特許番号
US04847305

関連ノート

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