Hydrochloric Acid → 3-(5-(2-(((4'-Chloro-[1,1'-biphenyl]-4-yl)amino)methyl)-6-(trifluoromethyl)phenyl)picolinamido)propanoic acid

HRID 405181ノート

反応式

HRID 405181 の反応式
[OH-].[Na+].C1COCC1.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][C:18]([NH:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([C:29]([F:32])([F:31])[F:30])[C:24]=3[C:33]3[CH:34]=[CH:35][C:36]([C:39]([NH:41][CH2:42][CH2:43][C:44]([O:46]CC)=[O:45])=[O:40])=[N:37][CH:38]=3)=[CH:17][CH:16]=2)=[CH:11][CH:10]=1.Cl>CO>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[CH:20]=[CH:19][C:18]([NH:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([C:29]([F:30])([F:32])[F:31])[C:24]=3[C:33]3[CH:34]=[CH:35][C:36]([C:39]([NH:41][CH2:42][CH2:43][C:44]([OH:46])=[O:45])=[O:40])=[N:37][CH:38]=3)=[CH:17][CH:16]=2)=[CH:13][CH:14]=1

参加物

6

実験手順

A 1M aqueous solution of NaOH (0.30 mL, 0.30 mmol) was added to a THF (0.6 mL) and MeOH (0.3 mL) solution of ethyl 3-(5-(2-(((4′-chloro-[1,1′-biphenyl]-4-yl)amino)methyl)-6-(trifluoromethyl)phenyl)picolinamido)propanoate (57.5 mg, 0.10 mmol) and the resulting homogeneous mixture was stirred at room temperature. After 45 min the resulting mixture was acidified with 1M HCl (0.31 mL, 0.31 mmol) and then extracted with DCM. The combined organics were dried (Na2SO4), concentrated and purified via column chromatography to yield the title compound.

後処理

  1. extractionextracted with DCM
  2. dry with materialThe combined organics were dried (Na2SO4)
  3. concentrationconcentrated
  4. custompurified via column chromatography

出典と根拠

ORDレコード
ord-882dde1a17004ef6a80b781ce4d4ab2d
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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