Methanesulfonic Acid → ethyl 3-[[2-[[4-[(Z)-N'-hexoxycarbonylcarbamimidoyl]anilino]methyl]-1-methylbenzimidazole-5-carbonyl]-pyridin-2-ylamino]propanoate;methanesulfonic acid

HRID 1470525Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1470525
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]([CH2:40][CH2:41][C:42]([O:44][CH2:45][CH3:46])=[O:43])[C:8]([C:10]1[CH:39]=[CH:38][C:13]2[N:14]([CH3:37])[C:15]([CH2:17][NH:18][C:19]3[CH:24]=[CH:23][C:22]([C:25](=[NH:36])[NH:26][C:27]([O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])=[O:28])=[CH:21][CH:20]=3)=[N:16][C:12]=2[CH:11]=1)=[O:9].[CH3:47][S:48]([OH:51])(=[O:50])=[O:49]>CC(C)=O>[CH3:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][O:29][C:27](/[N:26]=[C:25](\[NH2:36])/[C:22]1[CH:21]=[CH:20][C:19]([NH:18][CH2:17][C:15]2[N:14]([CH3:37])[C:13]3[CH:38]=[CH:39][C:10]([C:8]([N:7]([C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=4)[CH2:40][CH2:41][C:42]([O:44][CH2:45][CH3:46])=[O:43])=[O:9])=[CH:11][C:12]=3[N:16]=2)=[CH:24][CH:23]=1)=[O:28].[CH3:47][S:48]([OH:51])(=[O:50])=[O:49]

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 135565674Dabigatran Etexilate

Produkt 1

HCID 11434065ethyl 3-[[2-[[4-[(Z)-N'-hexoxycarbonylcarbamimidoyl]anilino]methyl]-1-methylbenzimidazole-5-carbonyl]-pyridin-2-ylamino]propanoate;methanesulfonic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel2×

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

100 g of 1-methyl-2-[N-[4-(N-n-hexyloxycarbonylamidino)phenyl]amino methyl]benzimidazol-5-yl-carboxylicacid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl) amide was dissolved in 890 ml of acetone under heating. A solution of 15 g of methane sulfonic acid in 200 ml of acetone was added to the reaction mixture. The solution is filtered and after the addition of 77 ml of acetone cooled to approximately 20° C. The precipitated product was filtered and washed with acetone then dried at 50° C. under reduced pressure.

Aufarbeitung

  1. temperatureunder heating
  2. filtrationThe solution is filtered
  3. additionafter the addition of 77 ml of acetone
  4. filtrationThe precipitated product was filtered
  5. washwashed with acetone
  6. customthen dried at 50° C. under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-00932948f0fe4086aff20bd266b58d45
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09006448B2

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