HCID 19754690、化合物 → 2-(3,3,5,5-Tetramethylcyclohexyl)phenylamine

HRID 604840ノート

反応式

HRID 604840 の反応式
[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

参加物

5

反応物 2

HCID 19754690HCID 19754690、化合物HCID 178418361HCID 178418361、化合物6 回

生成物 1

HCID 119922852-(3,3,5,5-Tetramethylcyclohexyl)phenylamine収率 96.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-487eecf69936401c8dc450f4424ac67a
出典データセット
uspto-grants-2011_03
特許番号
US07910734B2

反応ノート

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