2,4-Di-tert-butylphenol → Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-

HRID 277316

反応式

HRID 277316 の反応式
[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[CH:7][C:6]=1[OH:15])([CH3:4])([CH3:3])[CH3:2]>C(O)C.[Rh]>[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][C:6]1=[O:15])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 1

HCID 73112,4-Di-tert-butylphenol

生成物 1

HCID 114442Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-収率 91%

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒2 回HCID 702Ethanol溶媒

実験手順

410.0 g of 2,4-di-tert-butylphenol are hydrogenated in 820 ml of ethanol under 40 bar at 60° C. using 20 g of rhodium on carbon (5%) for 21 hours. To complete the reaction, the pressure is raised to 120 bar, a further 10 g of rhodium on carbon (5%) are added, and the hydrogenation is continued at 100° C. for 17 hours. The catalyst is filtered off, the solvent is distilled off under reduced pressure, and the residue is distilled off under high vacuum to leave 380.43 g (91% of theory) of 2,4-di-tert-butylcyclohexanone (mixed isomers) as a colourless liquid. Boiling point: 79-86° C./0.22 mbar.

後処理

  1. customfor 21 hours
  2. customthe reaction
  3. temperaturethe pressure is raised to 120 bar
  4. filtrationThe catalyst is filtered off
  5. distillationthe solvent is distilled off under reduced pressure
  6. distillationthe residue is distilled off under high vacuum

出典と根拠

ORDレコード
ord-1f2470bda4f04a2baa2ce6c00db94180
出典データセット
uspto-grants-2002_03
特許番号
US06355783B1

関連ノート

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