Oxalic Acid → 1-methyl-2[N-[4-amidinophenyl]aminomethyl]benzimidazol-5-yl-carboxylicacid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl)amide oxalate

HRID 1470514

Reaktionsgleichung

[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]([CH2:31][CH2:32][C:33]([O:35][CH2:36][CH3:37])=[O:34])[C:8]([C:10]1[CH:30]=[CH:29][C:13]2[N:14]([CH3:28])[C:15]([CH2:17][NH:18][C:19]3[CH:24]=[CH:23][C:22]([C:25](=[NH:27])[NH2:26])=[CH:21][CH:20]=3)=[N:16][C:12]=2[CH:11]=1)=[O:9].[C:38]([OH:43])(=[O:42])[C:39]([OH:41])=[O:40]>C(O)C>[C:38]([OH:43])(=[O:42])[C:39]([OH:41])=[O:40].[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]([CH2:31][CH2:32][C:33]([O:35][CH2:36][CH3:37])=[O:34])[C:8]([C:10]1[CH:30]=[CH:29][C:13]2[N:14]([CH3:28])[C:15]([CH2:17][NH:18][C:19]3[CH:24]=[CH:23][C:22]([C:25](=[NH:26])[NH2:27])=[CH:21][CH:20]=3)=[N:16][C:12]=2[CH:11]=1)=[O:9]

Komponenten

Reaktionsbedingungen

Temperatur: 55 °C

Versuchsvorschrift

A mixture of 1-methyl-2-[N-[4-amidinophenyl]aminomethyl]benzimidazol-5-yl-carboxylicacid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl)amide compound of formula-5 (100 g) and ethanol (1200 ml) was heated to 50-60° C. A solution of oxalic acid (25.25 g) in ethanol (1500 ml) was added to the above reaction mixture at 50-60° C. and stirred for 45 minutes. The reaction mixture was cooled to 25-35° C. and stirred for 6 hours at 25-35° C. Filtered the solid, washed with ethanol and then dried to get the title compound.

Aufarbeitung

temperatureThe reaction mixture was cooled to 25-35° C.
stirringstirred for 6 hours at 25-35° C
filtrationFiltered the solid
washwashed with ethanol
customdried

Quellen und Nachweise

ORD-Eintrag: ord-d548663fb9c64f02b3ede67f1688ca4a
Quelldatensatz: uspto-grants-2015_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09006448B2

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