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

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Reaktionsgleichung

[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

Komponenten

Reaktionsbedingungen

Temperatur: 40 °C

Versuchsvorschrift

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.

Aufarbeitung

extractionthe aqueous phase was extracted with EtOAc
washThe combined organics were washed with water
dry with materialdried (Na2SO4)
concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag: ord-83e44e24f5bb47d284f0b5247b5995bc
Quelldatensatz: uspto-grants-2014_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08748624B2

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