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

HRID 405230
ノート
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反応式

HRID 405230 の反応式
[Li+].[OH-].C1COCC1.[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([C:31](=[O:47])[NH:32][C:33]2[CH:38]=[CH:37][C:36]([C:39]3[CH:44]=[CH:43][C:42]([Cl:45])=[CH:41][C:40]=3[CH3:46])=[CH:35][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.Cl>CCOC(C)=O.O.CO>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([C:31](=[O:47])[NH:32][C:33]2[CH:38]=[CH:37][C:36]([C:39]3[CH:44]=[CH:43][C:42]([Cl:45])=[CH:41][C:40]=3[CH3:46])=[CH:35][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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 71059976Ethyl 3-(5-(5-chloro-2-((4'-chloro-2'-methyl-[1,1'-biphenyl]-4-yl)carbamoyl)phenyl)picolinamido)propanoate

生成物 1

HCID 710599323-(5-(5-Chloro-2-((4'-chloro-2'-methyl-[1,1'-biphenyl]-4-yl)carbamoyl)phenyl)picolinamido)propanoic acid

試薬・触媒・溶媒 3

HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A 1M aqueous solution of LiOH (2.0 mL, 2.0 mmol) was added to a THF (4.0 mL) and MeOH (1.0 mL) solution of ethyl 3-(5-(5-chloro-2-((4′-chloro-2′-methyl-[1,1′-biphenyl]-4-yl)carbamoyl)phenyl)picolinamido)propanoate (100 mg, 0.17 mmol) and the resulting mixture was stirred at room temperature. After 1 h the resulting mixture was neutralized with 2M aqueous HCl, diluted with EtOAc and water and the layers were separated. The aqueous layer was extracted with EtOAc and the combined extracts were dried (Na2SO4), and concentrated. The title compound was re-solidified from CH2Cl2/heptane (ca. 1/9) and dried in vacuo.

後処理

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted with EtOAc
  3. dry with materialthe combined extracts were dried (Na2SO4)
  4. concentrationconcentrated
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-b6a7aa61f2f248698c5cb9acce7768e8
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08748624B2

反応ノート

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