Hydrochloric Acid → Nilotinib Hydrochloride Anhydrous

HRID 1428264

반응식

HRID 1428264 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:39])([F:38])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[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.[ClH:40]>C(O)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:38])([F:39])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[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.[ClH:40]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 644241Nilotinib

생성물 1

HCID 16006490Nilotinib Hydrochloride Anhydrous

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
5 °C

실험 절차

Nilotinib HCl form T18 as used in any of the processes described in the present application may be prepared according to WO 2010/054056, examples 33-38, which is incorporated herein by reference. For example: To a 1 Liter reactor was added Nilotinib-base form A (20 g, 0.04 mol), absolute ethanol (188 ml) and 13.77% HCl solution in ethanol abs. (10 g, 0.04 mol). The slurry formed thereby was heated to reflux, and dissolution occurred during the stirring. The solution was then filtered under reduced pressure. The filtrate was fed back to the reactor and heated back to reflux. At 76.6° C. the solution was seeded with 0.2 g of dry material obtained by the process of example 23. Precipitation was observed. Then, the solution was maintained at reflux for 1 h, followed by cooling over 2 h to 6° C. At 6° C. ethanol abs. was added (300 ml) and the slurry was stirred at 5° C. for 30 minutes, filtered, washed with ethanol abs. to yield Nilotinib-HCl, form T18.

후처리

  1. custommay be prepared
  2. customThe slurry formed
  3. temperaturethereby was heated
  4. temperatureto reflux
  5. dissolutiondissolution
  6. filtrationThe solution was then filtered under reduced pressure
  7. temperatureheated back
  8. temperatureto reflux
  9. customAt 76.6° C.
  10. customobtained by the process of example 23
  11. customPrecipitation
  12. temperatureThen, the solution was maintained
  13. temperatureat reflux for 1 h
  14. temperatureby cooling over 2 h to 6° C
  15. customAt 6° C.
  16. additionwas added (300 ml)
  17. filtrationfiltered
  18. washwashed with ethanol abs

출처 및 근거

ORD 기록
ord-b0fc258ed38946c29f720d665d43e19c
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937082B2

연결된 노트

불러오는 중…