2-[4-(4-Chlorophenyl)phenyl]-5-ethyl-5-phenyl-1,3-dioxolan-4-one → 2-[4-(4-Chlorophenyl)benzyloxy]-2-phenylbutyric acid

HRID 1702540ノート

反応式

HRID 1702540 の反応式
[H][H].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([CH:16]3[O:20][C:19](=[O:21])[C:18]([CH2:28][CH3:29])([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[O:17]3)=[CH:12][CH:11]=2)=[CH:6][CH:5]=1>[Pd].C(O)C.C1(C)C=CC=CC=1>[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][O:17][C:18]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)([CH2:28][CH3:29])[C:19]([OH:21])=[O:20])=[CH:12][CH:11]=2)=[CH:6][CH:5]=1

参加物

6

反応物 2

HCID 127737622-[4-(4-Chlorophenyl)phenyl]-5-ethyl-5-phenyl-1,3-dioxolan-4-oneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 103397752-[4-(4-Chlorophenyl)benzyloxy]-2-phenylbutyric acid

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 1140Toluene溶媒

実験手順

Hydrogen gas was allowed to react with a stirred suspension of 2-[4-(4-chlorophenyl)phenyl]-5-ethyl-5-phenyl-1,3-dioxolan-4-one (3.8 g.) and 5% w/w palladium on carbon (0.2 g.) in ethanol (160 ml.) at 55° to 60° C. and atmospheric pressure for four hours. The mixture was diluted with toluene (50 ml.). The solid material was separated by filtration and the filtrate was evaporated. The resultant solid may be purified by high pressure liquid chromatography on "Spherisorb"* 5μ ODS solid phase using an eluant containing acetonitrile (62% v/v), water (37.9% v/v) and phosphoric acid (0.1% v/v) using ultraviolet absorbance at 262 μm for detection to give 2-[4-(4-chlorophenyl)benzyloxy]-2-phenylbutyric acid identical to that obtained in previous examples.

後処理

  1. customThe solid material was separated by filtration
  2. customthe filtrate was evaporated
  3. customThe resultant solid may be purified by high pressure liquid chromatography on "Spherisorb"* 5μ ODS solid phase
  4. additioncontaining acetonitrile (62% v/v), water (37.9% v/v) and phosphoric acid (0.1% v/v)

出典と根拠

ORDレコード
ord-d75311eeeefc4893bef64b87166c0a1a
出典データセット
uspto-grants-1982_09
特許番号
US04348322

反応ノート

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