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

HRID 619992

反応式

HRID 619992 の反応式
[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 66611,3-Dimethyl-2-imidazolidinone2 回HCID 14797Potassium HydroxideHCID 30671833-Chloro-4-ethoxyneophyl 3-phenoxybenzyl ether

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-4cf53a3e63ca4e588829b05f7f826fd5
出典データセット
uspto-grants-1989_04
特許番号
US04818525

関連ノート

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