Hydrochloric Acid → 3-Phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether

HRID 619992

반응식

HRID 619992 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:11]([CH3:29])([CH3:28])[CH2:12][O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:16]=2)[CH:5]=[CH:6][C:7]=1[O:8]CC.[OH-].[K+].CN1CCN(C)C1=O.Cl>O>[Cl:1][C:2]1[CH:3]=[C:4]([C:11]([CH3:29])([CH3:28])[CH2:12][O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH:16]=2)[CH:5]=[CH:6][C:7]=1[OH:8]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 66611,3-Dimethyl-2-imidazolidinone2회HCID 14797Potassium HydroxideHCID 30671833-Chloro-4-ethoxyneophyl 3-phenoxybenzyl ether

생성물 1

HCID 110580703-Phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether수율 48.9%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

100 g of 3-phenoxybenzyl 2-(3-chloro-4-ethoxyphenyl)-2-methylpropyl ether and 25 g of 97% potassium hydroxide were added to 300 ml of 1,3-dimethyl-2-imidazolidinone (hereinafter referred to as DMI) and the mixture was stirred at 150° C. for 18 h. After cooling to room temperature, the mixture was poured into water and made acidic with a concentrated aqueous hydrochloric acid solution. After extraction with benzene, the benzene solution was washed with water and dried. Benzene was distilled off under reduced pressure and the obtained oily residue was purified according to a column chromatography (silica gel, developer: benzene) to obtain 45.6 g of 3-phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether (m.p. 68° to 69° C.).

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionAfter extraction with benzene
  3. washthe benzene solution was washed with water
  4. customdried
  5. distillationBenzene was distilled off under reduced pressure
  6. customthe obtained oily residue was purified

출처 및 근거

ORD 기록
ord-4cf53a3e63ca4e588829b05f7f826fd5
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04818525

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