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

HRID 405270ノート

反応式

HRID 405270 の反応式
[OH-].[Na+].[Cl:3][C:4]1[CH:5]=[C:6]([C:25]2[CH:26]=[CH:27][C:28]([C:31]([NH:33][CH2:34][CH2:35][C:36]([O:38]CC)=[O:37])=[O:32])=[N:29][CH:30]=2)[CH:7]=[C:8]([CH2:10][NH:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=3)=[CH:14][CH:13]=2)[CH:9]=1.Cl>C1COCC1>[Cl:3][C:4]1[CH:5]=[C:6]([C:25]2[CH:26]=[CH:27][C:28]([C:31]([NH:33][CH2:34][CH2:35][C:36]([OH:38])=[O:37])=[O:32])=[N:29][CH:30]=2)[CH:7]=[C:8]([CH2:10][NH:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:19]=[CH:20][C:21]([F:24])=[CH:22][CH:23]=3)=[CH:14][CH:13]=2)[CH:9]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 71060021Ethyl 3-(5-(3-chloro-5-(((4'-fluoro-[1,1'-biphenyl]-4-yl)amino)methyl)phenyl)picolinamido)propanoate

生成物 1

HCID 710600783-(5-(3-Chloro-5-(((4'-fluoro-[1,1'-biphenyl]-4-yl)amino)methyl)phenyl)picolinamido)propanoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

A 1M aqueous solution of NaOH (0.47 mL, 0.47 mmol) was added to a THF solution (5 mL) of ethyl 3-(5-(3-chloro-5-(((4′-fluoro-[1,1′-biphenyl]-4-yl)amino)methyl)phenyl)picolinamido)propanoate (100 mg, 0.19 mmol) and the resulting mixture was heated to 40° C. After 4 h the resulting mixture was acidified with 1 M HCl and the aqueous phase was extracted with EtOAc. The combined organics were washed with water, dried (Na2SO4), and concentrated to yield the title compound.

後処理

  1. extractionthe aqueous phase was extracted with EtOAc
  2. washThe combined organics were washed with water
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-83e44e24f5bb47d284f0b5247b5995bc
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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