반응 #649745

반응 방정식

dioxolane

Imatinib

1,3-dioxolane

methanesulphonic acid

→

Imatinib Mesylate

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   workup.ADDITIONAfter addition the solution
3. 3
   온도was cooled from 20° C.-10° C. in 1 hour and after 1 hour
4. 4
   온도was cooled again from 10° C.-5° C. in 1 hour
5. 5
   workup.STIRRINGThe suspension was stirred for 4 hours at 5° C
6. 6
   workup.STIRRINGwithout stirring
7. 7
   여과The suspension was filtered
8. 8
   세척the product was washed with 6 liters of 1,3-dioxolane

실험 절차

Imatinib base (600 g), 5.7 liters of 1,3-dioxolane and 300 ml of water were added to a vessel. The suspension was stirred at 20° C. for 15 minutes and than 113.3 g of methanesulphonic acid was added. After addition the solution was cooled from 20° C.-10° C. in 1 hour and after 1 hour of stirring the solution was cooled again from 10° C.-5° C. in 1 hour. The suspension was stirred for 4 hours at 5° C. Than 6 liters of dioxolane was added in 30 minutes maintaining the temperature at 5° C. The suspension was left for 2.5 hours at 5° C. without stirring. The suspension was filtered and the product was washed with 6 liters of 1,3-dioxolane.

출처