HCID 19754690, 화합물 → 2-(3,3,5,5-Tetramethylcyclohexyl)phenylamine

HRID 604840노트

반응식

HRID 604840 반응식
[CH3:1][C:2]1([CH3:17])[CH2:7][C:6]([CH3:9])([CH3:8])[CH2:5][C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[NH2:16])=[CH:3]1.[H][H]>[Pd].C(O)C>[CH3:1][C:2]1([CH3:17])[CH2:7][C:6]([CH3:8])([CH3:9])[CH2:5][CH:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[NH2:16])[CH2:3]1

참가 물질

5

반응물 2

HCID 19754690HCID 19754690, 화합물HCID 178418361HCID 178418361, 화합물6회

생성물 1

HCID 119922852-(3,3,5,5-Tetramethylcyclohexyl)phenylamine수율 96.9%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

In a 100 mL autoclave, 10% palladium on carbon (water content 50%, 1.2 g) was added to a solution of 2-(3,3,5,5-tetramethylcyclohex-1-enyl)phenylamine (4.00 g, 17.4 mmol) in ethanol (40 mL), followed by stirring at room temperature, 5 kgf/cm2 of hydrogen pressure for 5.5 hours. Then the reaction mixture was stirred at room temperature, 10 kgf/cm2 of hydrogen pressure for 3 hours, introduction of hydrogen was stopped, and the reaction mixture was stirred at room temperature for 15 hours. The reaction mixture was stirred at room temperature, 10 kgf/cm2 of hydrogen pressure for 9.5 hours, introduction of hydrogen was stopped, and the reaction mixture was stirred at room temperature for 13 hours. The reaction mixture was stirred at room temperature, 10 kgf/cm2 of hydrogen pressure for 7.5 hours, and the reaction mixture was stirred at room temperature. The pressure was brought to atmospheric pressure, and the reaction mixture was filtered through Celite, and concentrated to give 3.90 g of the title compound as a brown oil.

후처리

  1. stirringThen the reaction mixture was stirred at room temperature
  2. stirringthe reaction mixture was stirred at room temperature for 15 hours
  3. stirringThe reaction mixture was stirred at room temperature
  4. stirringthe reaction mixture was stirred at room temperature for 13 hours
  5. stirringThe reaction mixture was stirred at room temperature
  6. stirringthe reaction mixture was stirred at room temperature
  7. filtrationthe reaction mixture was filtered through Celite
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-487eecf69936401c8dc450f4424ac67a
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07910734B2

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