4-Hydroxybiphenyl → HCID 178521548, 화합물

HRID 1388245

반응식

HRID 1388245 반응식
[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

참가 물질

5

반응물 2

HCID 71034-HydroxybiphenylHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 178521548HCID 178521548, 화합물수율 19.3%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-44696fcaef4f4b81821101fb2da0fa4c
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04431564

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