반응 #640612

ord-5cc0358765cf4de4956c0e8344c30b49

반응 방정식

Cc1ccc(NC(=O)c2ccc(CN3CCN(C)CC3)cc2)cc1Nc1nccc(-c2cccnc2)n1
Imatinib
CS(=O)(=O)O
methane sulfonic acid
CS(=O)(=O)O.Cc1ccc(NC(=O)c2ccc(CN3CCN(C)CC3)cc2)cc1Nc1nccc(-c2cccnc2)n1
Imatinib mesylate

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도under reflux for 20 minutes
  3. 3
    여과than filtered at 65° C
  4. 4
    기타The filtrate was evaporated down to 50%
  5. 5
    여과the residue filtered off at 25° C.
  6. 6
    여과(filter material A)
  7. 7
    기타The mother liquor was evaporated to dryness
  8. 8
    여과The residue and filter material A
  9. 9
    workup.DISSOLUTIONdissolved
  10. 10
    온도under reflux with addition of water
  11. 11
    온도Cooling
  12. 12
    여과overnight to 25° C., filtration
  13. 13
    기타drying

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08048883B2uspto-grants-2011_11