Reaktion #2507851

Reaktionsgleichung

Eltrombopag

Ethanolamine

ethanolamine

Water

→

title compound

Ausbeute 96.0%

Eltrombopag ethanolamine

Ausbeute 96.0%

Lösungsmittel

THF

—

IMS

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto maintain a temperature greater
2. 2
   Sonstige28° C
3. 3
   workup.ADDITIONWhen addition
4. 4
   Sonstigewas returned to 30° C.
5. 5
   Filtrationthe solution filtered through a glass fiber pad (2× Whatman GFC filters)
6. 6
   Sonstigeto remove particulate matter
7. 7
   WaschenThe filter was washed through with THF (2.0 ml) which
8. 8
   workup.ADDITIONwas added to the filtrate
9. 9
   workup.ADDITIONThe filtrate containing the free acid
10. 10
    workup.STIRRINGThe resulting dark red suspension was stirred for 3 hours
11. 11
    Sonstigethe solid isolated by filtration
12. 12
    Sonstigedried at 50° C. in a vacuum oven over night

Vorschrift

Eltrombopag crude orange solid (1 g) was stirred in 16.75 ml of THF at approximately 30° C. Water (2.0 ml) was added slowly so as to maintain a temperature greater then 28° C. When addition was complete, the temperature was returned to 30° C. and the solution filtered through a glass fiber pad (2× Whatman GFC filters) to remove particulate matter. The filter was washed through with THF (2.0 ml) which was added to the filtrate. The filtrate was allowed to cool to room temperature. Ethanolamine (0.324 g, 2.35 mol. equiv.) was dissolved in IMS (26 ml) at 22° C. and stirred under a nitrogen atmosphere at 22° C. The filtrate containing the free acid was added to the ethanolamine solution over 20 to 30 minutes. The resulting dark red suspension was stirred for 3 hours and the solid isolated by filtration and dried at 50° C. in a vacuum oven over night to yield 1.22 g (96%) of the title compound.

Quelle