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Water → 3-(4-Fluorophenethyl)-6-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]pyridin-2-carboxylic acid

HRID 1251923
ノート
印刷プレビュー

反応式

HRID 1251923 の反応式
[F:1][C:2]1[CH:35]=[CH:34][C:5]([CH2:6][CH2:7][C:8]2[C:9]([C:30]([O:32]C)=[O:31])=[N:10][C:11]([O:14][CH:15]([C:23]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=3)[CH2:16][C:17]3[N:21]([CH3:22])[CH:20]=[N:19][CH:18]=3)=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.[OH-].[Na+].O>CO>[F:1][C:2]1[CH:35]=[CH:34][C:5]([CH2:6][CH2:7][C:8]2[C:9]([C:30]([OH:32])=[O:31])=[N:10][C:11]([O:14][CH:15]([C:23]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=3)[CH2:16][C:17]3[N:21]([CH3:22])[CH:20]=[N:19][CH:18]=3)=[CH:12][CH:13]=2)=[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 962WaterHCID 14798Sodium HydroxideHCID 18324461Methyl 3-(4-fluorophenethyl)-6-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]pyridin-2-carboxylate

生成物 1

HCID 183243783-(4-Fluorophenethyl)-6-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]pyridin-2-carboxylic acid収率 80.6%

試薬・触媒・溶媒 1

HCID 887Methanol
溶媒

実験手順

A mixture of methyl 3-(4-fluorophenethyl)-6-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]pyridin-2-carboxylate (1.56 g), sodium hydroxide (0.65 g), water (12 ml) and methanol (80 ml) was heated at reflux for 16 hours and then cooled to ambient temperature. The mixture was concentrated under reduced pressure, 1M citric acid (17 ml) added and the mixture extracted with 10% methanol/dichloromethane (1×50 ml, 2×30 ml). The extracts were dried and concentrated under reduced pressure to give 3-(4-fluorophenethyl)-6-[1-(4-fluorophenyl)-2-(1-methylimidazol-5-yl)ethoxy]pyridin-2-carboxylic acid as a pale yellow foam (1.22 g).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 16 hours
  3. concentrationThe mixture was concentrated under reduced pressure, 1M citric acid (17 ml)
  4. additionadded
  5. extractionthe mixture extracted with 10% methanol/dichloromethane (1×50 ml, 2×30 ml)
  6. customThe extracts were dried
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b242954fa7044c409f4f0a30a0fa1f35
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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