Reaktion #42065

Reaktionsgleichung

4-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethyl-N-{4-methyl-3-[4-(3-pyridyl)pyridin-2-ylamino]phenyl}benzamide

methanesulfonic acid

→

objective compound

4-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethyl-N-{4-methyl-3-[4-(3-pyridyl)pyridin-2-ylamino]phenyl}benzamide methanesulfonate

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwith heating
2. 2
   SonstigeInsolubles were removed by filtration
3. 3
   Temperaturwith heating
4. 4
   workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
5. 5
   SonstigeThe residue was crystallized
6. 6
   workup.ADDITIONby adding isopropanol
7. 7
   Filtrationcollected by filtration

Vorschrift

1.21 g of 4-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethyl-N-{4-methyl-3-[4-(3-pyridyl)pyridin-2-ylamino]phenyl}benzamide (Example 28) was suspended in 20 ml of methanol and 140 μl of methanesulfonic acid was added, followed by stirring with heating. Insolubles were removed by filtration with heating and the solvent in the filtrate was distilled off under reduced pressure. The residue was crystallized by adding isopropanol and collected by filtration to obtain 1.33 g of the objective compound as pale yellow crystals.

Quelle