Hydrochloric Acid → AM-432

HRID 1625669노트

반응식

HRID 1625669 반응식
C([O:3][C:4](=[O:38])[CH2:5][C:6]1[CH:7]=[C:8]([C:14]2[CH:19]=[CH:18][C:17]([C:20]3[CH:21]=[N:22][C:23]([O:26][CH2:27][CH3:28])=[CH:24][CH:25]=3)=[CH:16][C:15]=2[CH2:29][N:30]([C:33]([CH:35]2[CH2:37][CH2:36]2)=[O:34])[CH2:31][CH3:32])[C:9]([O:12][CH3:13])=[CH:10][CH:11]=1)C.[OH-].[Li+].Cl>O1CCCC1.O>[CH:35]1([C:33]([N:30]([CH2:29][C:15]2[CH:16]=[C:17]([C:20]3[CH:21]=[N:22][C:23]([O:26][CH2:27][CH3:28])=[CH:24][CH:25]=3)[CH:18]=[CH:19][C:14]=2[C:8]2[C:9]([O:12][CH3:13])=[CH:10][CH:11]=[C:6]([CH2:5][C:4]([OH:38])=[O:3])[CH:7]=2)[CH2:31][CH3:32])=[O:34])[CH2:36][CH2:37]1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 58149167[2'-[(Cyclopropanecarbonyl-ethyl-amino)-methyl]-4'-(6-ethoxy-pyridin-3-yl)-6-methoxy-biphenyl-3-yl]-acetic acid ethyl ester

생성물 1

HCID 50901658AM-432

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

[2′-[(Cyclopropanecarbonyl-ethyl-amino)-methyl]-4′-(6-ethoxy-pyridin-3-yl)-6-methoxy-biphenyl-3-yl]-acetic acid ethyl ester (0.296 g, 0.573 mmol) in tetrahydrofuran (5 mL) and water was treated with lithium hydroxide (0.090 g, 2.14 mmol) and the reaction was stirred at room temperature. When the reaction was complete by analytical LCMS, the mixture was acidified with 1N aqueous hydrochloric acid and extracted three times with ethyl acetate. The combined organic layers were dried and concentrated, and the residue was purified by preparative HPLC to give the title compound.

후처리

  1. extractionextracted three times with ethyl acetate
  2. customThe combined organic layers were dried
  3. concentrationconcentrated
  4. customthe residue was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-5500dd54098e49a19d75764d125ccc1a
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785393B2

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