Majantol → 2,2-Dimethyl-3-(3-methylcyclohexyl)propan-1-ol

HRID 2369785

반응식

HRID 2369785 반응식
[CH3:1][C:2]([CH3:13])([CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH3:12])[CH:7]=1)[CH2:3][OH:4]>O.[Rh]>[CH3:1][C:2]([CH3:13])([CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH:8]([CH3:12])[CH2:7]1)[CH2:3][OH:4]

참가 물질

4

반응물 1

HCID 175948Majantol

생성물 1

HCID 574294222,2-Dimethyl-3-(3-methylcyclohexyl)propan-1-ol수율 82%

시약·촉매·용매 2

HCID 23948Rhodium촉매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

5% Rh/C (450 mg, 15% w/w) was charged into a 50 mL autoclave vessel containing a mixture of 2,2-dimethyl-3-(3-methylphenyl)propan-1-ol (6 g, 34 mmol) in water (17 mL). The mixture was vigorously stirred under an hydrogen atmosphere (10 Bar) at 60° C. for 6 h. The reaction mixture was filtered and the filtrate was extracted with MTBE (25 mL), dried over magnesium sulphate and concentrated. The resulting crude product was distilled with a bulb-to-bulb distillation (2.5 mBar, 90° C.) to give 2,2-dimethyl-3-(3-methylcyclohexyl)propan-1-ol (5.1 g, gc purity>99%; yield 82%).

후처리

  1. additioncontaining
  2. filtrationThe reaction mixture was filtered
  3. extractionthe filtrate was extracted with MTBE (25 mL)
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated
  6. distillationThe resulting crude product was distilled with a bulb-to-bulb distillation (2.5 mBar, 90° C.)

출처 및 근거

ORD 기록
ord-beb4fec26d5f494e9bee0fa0dfd974a8
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08709994B2

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