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

HRID 405130ノート

反応式

HRID 405130 の反応式
[OH-].[Na+].C1COCC1.[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:31][NH:32][C:33]2[CH:38]=[CH:37][C:36]([C:39]3[CH:44]=[CH:43][C:42]([Cl:45])=[CH:41][CH:40]=3)=[C:35]([Cl:46])[CH:34]=2)=[C:13]([C:15]2[CH:16]=[CH:17][C:18]([C:21]([NH:23][CH2:24][CH2:25][C:26]([O:28]CC)=[O:27])=[O:22])=[N:19][CH:20]=2)[CH:14]=1>CO>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:31][NH:32][C:33]2[CH:38]=[CH:37][C:36]([C:39]3[CH:40]=[CH:41][C:42]([Cl:45])=[CH:43][CH:44]=3)=[C:35]([Cl:46])[CH:34]=2)=[C:13]([C:15]2[CH:16]=[CH:17][C:18]([C:21]([NH:23][CH2:24][CH2:25][C:26]([OH:28])=[O:27])=[O:22])=[N:19][CH:20]=2)[CH:14]=1

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 71059870Ethyl 3-(5-(5-chloro-2-(((2,4'-dichloro-[1,1'-biphenyl]-4-yl)amino)methyl)phenyl)picolinamido)propanoate

生成物 1

HCID 710600203-(5-(5-Chloro-2-(((2,4'-dichloro-[1,1'-biphenyl]-4-yl)amino)methyl)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 (6.5 mL, 22.6 mmol) was added to a THF (10 mL) and MeOH (5 mL) solution of ethyl 3-(5-(5-chloro-2-(((2,4′-dichloro-[1,1′-biphenyl]-4-yl)amino)methyl)phenyl)picolinamido)propanoate (3.8 g, 6.5 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-fdb4cfc95d4343a5b71a78a1c80211b4
出典データセット
uspto-grants-2014_06
特許番号
US08748624B2

反応ノート

読み込み中…