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

HRID 277316

반응식

HRID 277316 반응식
[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]

참가 물질

4

반응물 1

HCID 73112,4-Di-tert-butylphenol

생성물 1

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

시약·촉매·용매 2

HCID 23948Rhodium촉매2회HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1f2470bda4f04a2baa2ce6c00db94180
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355783B1

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