p-Toluenesulfonate → Sorafenib Tosylate

HRID 332936

Reaktionsgleichung

Reaktionsgleichung von HRID 332936
[S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)([O-:4])(=[O:3])=[O:2].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([NH:22][C:23]2[CH:39]=[CH:38][C:26]([O:27][C:28]3[CH:33]=[CH:32][N:31]=[C:30]([C:34]([NH:36][CH3:37])=[O:35])[CH:29]=3)=[CH:25][CH:24]=2)=[O:21])=[CH:15][C:14]=1[C:40]([F:43])([F:42])[F:41]>CO>[S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)([OH:4])(=[O:3])=[O:2].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([NH:22][C:23]2[CH:39]=[CH:38][C:26]([O:27][C:28]3[CH:33]=[CH:32][N:31]=[C:30]([C:34]([NH:36][CH3:37])=[O:35])[CH:29]=3)=[CH:25][CH:24]=2)=[O:21])=[CH:15][C:14]=1[C:40]([F:43])([F:41])[F:42]

Komponenten

4

Edukt 2

HCID 85570p-ToluenesulfonateHCID 216239Sorafenib

Produkt 1

HCID 406563Sorafenib Tosylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

3.5 g of the tosylate salt of 4-{4-[({[4-chloro-3-(trifluoromethyl)phenyl]amino}carbonyl)-amino]phenoxy}-N-methylpyridine-2-carboxamide in the polymorph II are suspended in 15 ml of methanol and stirred at room temperature. After one week, the suspension is filtered and the residue dried at room temperature. Subsequently, the product is heat-treated at 150° C. for 30 min. The residue is analyzed by X-ray diffractometry and corresponds to the title compound in the polymorph III.

Aufarbeitung

  1. waitAfter one week
  2. filtrationthe suspension is filtered
  3. customthe residue dried at room temperature
  4. additionSubsequently, the product is heat-treated at 150° C. for 30 min

Quellen und Nachweise

ORD-Eintrag
ord-21e034fe98d94e6bb1f2b10d3807ccd0
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08877933B2

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