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

HRID 489990
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HRID 489990 반응식
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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-c7205a9424ce4f5b82848f856297293b
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06979692B2

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