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

HRID 1054648ノート

反応式

HRID 1054648 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 1 N 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 1 N 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-a8a8799fcbd141cb828bcccc302835e2
出典データセット
uspto-grants-2016_07
特許番号
US09394285B2

反応ノート

読み込み中…