反応 #42065

反応方程式

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

溶媒

methanol

反応条件

後処理

1. 1
   温度with heating
2. 2
   その他Insolubles were removed by filtration
3. 3
   温度with heating
4. 4
   workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
5. 5
   その他The residue was crystallized
6. 6
   workup.ADDITIONby adding isopropanol
7. 7
   ろ過collected by filtration

実験手順

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.

出典