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Methanol → 2-(4-Fluorophenethyl)-5-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]benzoic acid

HRID 1251910
ノート
印刷プレビュー

反応式

HRID 1251910 の反応式
[F:1][C:2]1[CH:34]=[CH:33][C:5]([CH2:6][CH2:7][C:8]2[CH:16]=[CH:15][C:14]([O:17][CH:18]([C:26]3[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=3)[CH2:19][C:20]3[N:24]([CH3:25])[CH:23]=[N:22][CH:21]=3)=[CH:13][C:9]=2[C:10]([O-:12])=[O:11])=[CH:4][CH:3]=1.[OH-].[Na+].CO>O>[F:1][C:2]1[CH:34]=[CH:33][C:5]([CH2:6][CH2:7][C:8]2[CH:16]=[CH:15][C:14]([O:17][CH:18]([C:26]3[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=3)[CH2:19][C:20]3[N:24]([CH3:25])[CH:23]=[N:22][CH:21]=3)=[CH:13][C:9]=2[C:10]([OH:12])=[O:11])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 183243882-(4-Fluorophenethyl)-5-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]benzoate

生成物 1

HCID 183243842-(4-Fluorophenethyl)-5-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]benzoic acid収率 73.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2-(4-fluorophenethyl)-5-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]benzoate (1.5 g.), sodium hydroxide (0.62 g.), methanol (200 ml.) and water (30 ml.) was stirred at reflux for 16 hours. The mixture was then cooled, the methanol evaporated away and the residue diluted with water (100 ml.). It was then washed with dichloromethane and the aqueous phase separated, acidified with 1M aqueous citric acid (25 ml.) and extracted with dichloromethane. The extracts were dried and evaporated to dryness to give 2-(4-fluorophenethyl)-5-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]benzoic acid as a white foam (1.1 g).

後処理

  1. temperatureat reflux for 16 hours
  2. temperatureThe mixture was then cooled
  3. customthe methanol evaporated away
  4. additionthe residue diluted with water (100 ml.)
  5. washIt was then washed with dichloromethane
  6. customthe aqueous phase separated
  7. extractionextracted with dichloromethane
  8. customThe extracts were dried
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-0c693c2a60c24fb5894068df55f0fe86
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06342765B1

反応ノート

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