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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
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HRID 405230 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 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

생성물 1

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

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b6a7aa61f2f248698c5cb9acce7768e8
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08748624B2

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