Tetrahydrofuran → 3-(5-(2-(((2,4'-Dichloro-2'-methyl-[1,1'-biphenyl]-4-yl)amino)methyl)-5-(trifluoromethyl)phenyl)picolinamido)propanoic acid

HRID 405158ノート

反応式

HRID 405158 の反応式
[OH-].[Na+].C1COCC1.[Cl:8][C:9]1[CH:14]=[C:13]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:19][C:18]=2[C:27]2[CH:28]=[CH:29][C:30]([C:33]([NH:35][CH2:36][CH2:37][C:38]([O:40]CC)=[O:39])=[O:34])=[N:31][CH:32]=2)[CH:12]=[CH:11][C:10]=1[C:43]1[CH:48]=[CH:47][C:46]([Cl:49])=[CH:45][C:44]=1[CH3:50]>CO>[Cl:8][C:9]1[CH:14]=[C:13]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:24])([F:26])[F:25])=[CH:19][C:18]=2[C:27]2[CH:28]=[CH:29][C:30]([C:33]([NH:35][CH2:36][CH2:37][C:38]([OH:40])=[O:39])=[O:34])=[N:31][CH:32]=2)[CH:12]=[CH:11][C:10]=1[C:43]1[CH:48]=[CH:47][C:46]([Cl:49])=[CH:45][C:44]=1[CH3:50]

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 71060055Ethyl 3-(5-(2-(((2,4'-dichloro-2'-methyl-[1,1'-biphenyl]-4-yl)amino)methyl)-5-(trifluoromethyl)phenyl)picolinamido)propanoate

生成物 1

HCID 710598553-(5-(2-(((2,4'-Dichloro-2'-methyl-[1,1'-biphenyl]-4-yl)amino)methyl)-5-(trifluoromethyl)phenyl)picolinamido)propanoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 3M aqueous solution of NaOH (5.6 mL, 16.7 mmol) was added to a THF (20 mL) and MeOH (10 mL) solution of ethyl 3-(5-(2-(((2,4′-dichloro-2′-methyl-[1,1′-biphenyl]-4-yl)amino)methyl)-5-(trifluoromethyl)phenyl)picolinamido)propanoate (3.5 g, 5.6 mmol) and the resulting homogeneous mixture was stirred at room temperature. After 16 h the resulting mixture was concentrated in vacuo, suspended in water, and acidified with 2 M HCl. The resulting precipitate was filtered off, dried in vacuo, and purified via HPLC to yield the title compound.

後処理

  1. concentrationAfter 16 h the resulting mixture was concentrated in vacuo
  2. filtrationThe resulting precipitate was filtered off
  3. customdried in vacuo
  4. custompurified via HPLC

出典と根拠

ORDレコード
ord-bab2d4a172fe47c693bc42ae3c8777ad
出典データセット
uspto-grants-2014_06
特許番号
US08748624B2

反応ノート

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