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

HRID 2369785

反応式

HRID 2369785 の反応式
[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]

参加物

4

反応物 1

HCID 175948Majantol

生成物 1

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

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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%).

後処理

  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.)

出典と根拠

ORDレコード
ord-beb4fec26d5f494e9bee0fa0dfd974a8
出典データセット
uspto-grants-2014_04
特許番号
US08709994B2

関連ノート

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