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

HRID 231589

반응식

HRID 231589 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-eb54f59a4b2e411eb36221891cf989dc
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04847305

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