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Lithium hydroxide, monohydrate → 1-Ethyl-5-[(4'-trifluoromethyl-biphenyl-2-carbonyl)-amino]-1H-indole-2-carboxylic acid

HRID 1455824
ノート
印刷プレビュー

反応式

HRID 1455824 の反応式
C([O:3][C:4]([C:6]1[N:7]([CH2:34][CH3:35])[C:8]2[C:13]([CH:14]=1)=[CH:12][C:11]([NH:15][C:16]([C:18]1[C:19]([C:24]3[CH:29]=[CH:28][C:27]([C:30]([F:33])([F:32])[F:31])=[CH:26][CH:25]=3)=[CH:20][CH:21]=[CH:22][CH:23]=1)=[O:17])=[CH:10][CH:9]=2)=[O:5])C.O.[OH-].[Li+]>CO.O>[CH2:34]([N:7]1[C:8]2[C:13](=[CH:12][C:11]([NH:15][C:16]([C:18]3[C:19]([C:24]4[CH:29]=[CH:28][C:27]([C:30]([F:32])([F:33])[F:31])=[CH:26][CH:25]=4)=[CH:20][CH:21]=[CH:22][CH:23]=3)=[O:17])=[CH:10][CH:9]=2)[CH:14]=[C:6]1[C:4]([OH:5])=[O:3])[CH3:35]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 12148798ethyl 1-ethyl-5-({2-[4-(trifluoromethyl)phenyl]benzene}amido)-1H-indole-2-carboxylate

生成物 1

HCID 121487951-Ethyl-5-[(4'-trifluoromethyl-biphenyl-2-carbonyl)-amino]-1H-indole-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

1-Ethyl-5-[(4′-trifluoromethyl-biphenyl-2-carbonyl)-amino]-1H-indole-2-carboxylic acid ethyl ester (4.5 g, 9.37 mmol) was added to MeOH/H2O (110 mL, 10/1). Lithium hydroxide monohydrate (1.5 g, 35.7 mmol) was added to the above mixture. The mixture which resulted was heated to reflux overnight. The solvent was removed under reduced pressure and the residue was dissolved in H2O (500 mL). The solution was acidified with 6N HCl to pH 2. The solid was collected by filtration and dried under vacuum (4.0 g, 94.5%).

後処理

  1. customThe mixture which resulted
  2. temperaturewas heated
  3. temperatureto reflux overnight
  4. customThe solvent was removed under reduced pressure
  5. dissolutionthe residue was dissolved in H2O (500 mL)
  6. filtrationThe solid was collected by filtration
  7. customdried under vacuum (4.0 g, 94.5%)

出典と根拠

ORDレコード
ord-8e0856cd796f4319ab6c60590250fc0e
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482368B2

反応ノート

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