Reaction #640612

Reaction equation

Imatinib

methane sulfonic acid

→

Imatinib mesylate

Solvents

ethanol

Conditions

Workup

1. 1
   Temperatureheated
2. 2
   Temperatureunder reflux for 20 minutes
3. 3
   Filtrationthan filtered at 65° C
4. 4
   OtherThe filtrate was evaporated down to 50%
5. 5
   Filtrationthe residue filtered off at 25° C.
6. 6
   Filtration(filter material A)
7. 7
   OtherThe mother liquor was evaporated to dryness
8. 8
   FiltrationThe residue and filter material A
9. 9
   workup.DISSOLUTIONdissolved
10. 10
    Temperatureunder reflux with addition of water
11. 11
    TemperatureCooling
12. 12
    Filtrationovernight to 25° C., filtration
13. 13
    Otherdrying

Procedure

Imatinib base was suspended in ethanol, methane sulfonic acid was added and heated under reflux for 20 minutes and than filtered at 65° C. The filtrate was evaporated down to 50% and the residue filtered off at 25° C. (filter material A). The mother liquor was evaporated to dryness. The residue and filter material A were suspended in ethanol dissolved under reflux with addition of water. Cooling overnight to 25° C., filtration and drying yielded Imatinib mesylate α-crystal form.

Source