Sodium Hydroxide → Phenol, 4-(1,1-dimethyl-2-((3-phenoxyphenyl)methoxy)ethyl)-

HRID 619993노트

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HRID 619993 반응식
Cl[C:2]1[CH:3]=[C:4]([C:9]([CH3:27])([CH3:26])[CH2:10][O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH:14]=2)[CH:5]=[CH:6][C:7]=1[OH:8].[OH-].[Na+]>[Pd].CO>[OH:8][C:7]1[CH:2]=[CH:3][C:4]([C:9]([CH3:27])([CH3:26])[CH2:10][O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[CH:14]=2)=[CH:5][CH:6]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 110580703-Phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether

생성물 1

HCID 157700Phenol, 4-(1,1-dimethyl-2-((3-phenoxyphenyl)methoxy)ethyl)-수율 100%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

반응 조건

온도
100 °C

실험 절차

20.0 g of 3-phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether prepared in the above step (1), 2.67 g of 95% sodium hydroxide and 1.0 g of 5% Pd-C (50% hydrous) were added to 100 ml of 80% methanol and the mixture was stirred at 100° C. under a hydrogen pressure of 20 to 30 kg/cm2G for 6 h. After cooling, the catalyst was removed by filtration and the catalyst was washed thoroughly with benzene. The solvent was distilled off under reduced pressure. A dilute aqueous hydrochloric acid solution was added to the distillation residue. After extraction with benzene, the benzene solution was washed with water and dried. Benzene was distilled off under reduced pressure to obtain 18.2 g of intended 3-phenoxybenzyl 2-(4-hydroxyphenyl)-2-methylpropyl ether (m.p. 69.2° to 70.0° C.).

후처리

  1. temperatureAfter cooling
  2. customthe catalyst was removed by filtration
  3. washthe catalyst was washed thoroughly with benzene
  4. distillationThe solvent was distilled off under reduced pressure
  5. additionA dilute aqueous hydrochloric acid solution was added to the distillation residue
  6. extractionAfter extraction with benzene
  7. washthe benzene solution was washed with water
  8. customdried
  9. distillationBenzene was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-7a29f7acb0ec4f2f8a957c1b50d0d18d
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04818525

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