Potassium Hydroxide → 6-Chloro-5-(4-ethoxyphenyl)-1H-indole-3-carboxylic acid

HRID 338304ノート

反応式

HRID 338304 の反応式
ClC(Cl)(Cl)[C:3]([C:5]1[C:13]2[C:8](=[CH:9][C:10]([Cl:23])=[C:11]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH3:22])=[CH:16][CH:15]=3)[CH:12]=2)[NH:7][CH:6]=1)=[O:4].[OH-:26].[K+]>COCCOC>[Cl:23][C:10]1[CH:9]=[C:8]2[C:13]([C:5]([C:3]([OH:26])=[O:4])=[CH:6][NH:7]2)=[CH:12][C:11]=1[C:14]1[CH:15]=[CH:16][C:17]([O:20][CH2:21][CH3:22])=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 866986512,2,2-trichloro-1-(6-chloro-5-(4-ethoxyphenyl)-1H-indol-3-yl)ethanone

生成物 1

HCID 866986506-Chloro-5-(4-ethoxyphenyl)-1H-indole-3-carboxylic acid収率 70%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of 2,2,2-trichloro-1-(6-chloro-5-(4-ethoxyphenyl)-1H-indol-3-yl)ethanone (70.0 mg, 0.17 mmol) in DME (1 mL) was added 1N KOH (0.71 mmol, 0.71 mL). The reaction mixture was stirred at room temperature for 12 hours, and concentrated in vacuo. The crude material was diluted with water (5 mL), and acidified to pH 2.5 with 1N HCl to form a white precipitate. The precipitate was filtered, washed with water (20 mL) and dried under vacuum to provide the title compound (37 mg, 70%) as an off-white solid.

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe crude material was diluted with water (5 mL)
  3. customto form a white precipitate
  4. filtrationThe precipitate was filtered
  5. washwashed with water (20 mL)
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-244b849b38114008911dcfe7b3109046
出典データセット
uspto-grants-2014_11
特許番号
US08889730B2

反応ノート

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