4-Hydroxybiphenyl → HCID 178521548、化合物

HRID 1388245

反応式

HRID 1388245 の反応式
[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H][H]>C(O)C.[Ni]>[C:1]1([C@H:7]2[CH2:8][CH2:9][C@H:10]([OH:13])[CH2:11][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 2

HCID 71034-HydroxybiphenylHCID 178418361HCID 178418361、化合物

生成物 1

HCID 178521548HCID 178521548、化合物収率 19.3%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

p-Phenylphenol (VI) (1 kg, 5.88 mols) dissolved in ethanol (2 l) was fed into a 5 l autoclave, and hydrogenation reaction was carried out at a reaction temperature of 150° to 160° C. under a hydrogen pressure of 30 to 40 kg/cm2 using a developed Raney nickel (100 g) as catalyst. When 17.6 mols of hydrogen were absorbed, the reaction was stopped. After cooling, the catalyst was filtered off, and the filtrate was concentrated to remove ethanol. The resulting residue was dissolved in toluene. The toluene solution was washed a few times with 2 N--NaOH aqueous solution and further with water, and toluene was then removed by concentration of the solution. The resulting raw crystals were recrystallized from ethanol to obtain trans-4-phenylcyclohexanol (VII) (200 g) having a melting point of 118.4°-119.2° C.

後処理

  1. customwas fed into a 5 l autoclave, and hydrogenation reaction
  2. customwas carried out at a reaction temperature of 150° to 160° C. under a hydrogen
  3. temperatureAfter cooling
  4. filtrationthe catalyst was filtered off
  5. concentrationthe filtrate was concentrated
  6. customto remove ethanol
  7. dissolutionThe resulting residue was dissolved in toluene
  8. washThe toluene solution was washed a few times with 2 N
  9. customNaOH aqueous solution and further with water, and toluene was then removed by concentration of the solution
  10. customThe resulting raw crystals were recrystallized from ethanol

出典と根拠

ORDレコード
ord-44696fcaef4f4b81821101fb2da0fa4c
出典データセット
uspto-grants-1984_02
特許番号
US04431564

関連ノート

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