Imatinib → Imatinib Mesylate

HRID 553430Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 553430
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([NH:21][C:22]([C:24]2[CH:25]=[CH:26][C:27]([CH2:30][N:31]3[CH2:36][CH2:35][N:34]([CH3:37])[CH2:33][CH2:32]3)=[CH:28][CH:29]=2)=[O:23])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]>C(O)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([NH:21][C:22]([C:24]2[CH:29]=[CH:28][C:27]([CH2:30][N:31]3[CH2:32][CH2:33][N:34]([CH3:37])[CH2:35][CH2:36]3)=[CH:26][CH:25]=2)=[O:23])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]

Komponenten

4

Edukt 2

HCID 5291ImatinibHCID 6395Methanesulfonic Acid

Produkt 1

HCID 123596Imatinib Mesylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 20 minutes
  3. filtrationthan filtered at 65° C
  4. customThe filtrate was evaporated down to 50%
  5. filtrationthe residue filtered off at 25° C.
  6. filtration(filter material A)
  7. customThe mother liquor was evaporated to dryness
  8. filtrationThe residue and filter material A
  9. dissolutiondissolved
  10. temperatureunder reflux with addition of water
  11. temperatureCooling
  12. filtrationovernight to 25° C., filtration
  13. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-5cc0358765cf4de4956c0e8344c30b49
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08048883B2

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