Hydrochloric Acid → Nilotinib Hydrochloride Anhydrous

HRID 2368541Notes

Reaction equation

HRID 2368541 reaction equation
[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]>CC(O)(CC)C.C(OCC)(=O)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:29]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:27]=[C:26]([C:36]([F:37])([F:39])[F:38])[CH:25]=2)=[O:22])=[CH:6][C:7]=1[NH:8][C:9]1[N:14]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[CH:12]=[CH:11][N:10]=1.[ClH:40]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 644241Nilotinib

Product 1

HCID 16006490Nilotinib Hydrochloride Anhydrous

Reagents, catalysts & solvents 2

HCID 64052-Methyl-2-butanolSolventHCID 8857Ethyl AcetateSolvent

Conditions

Temperature
70 °C

Procedure

Nilotinib (3 gm) was suspended in 2-methyl-2-butanol (120 ml) and then heated to 70° C. A solution of hydrochloric acid in ethyl acetate (4 ml) was added to the solution at 70° C. The solution was stirred for 30 minutes at 70° C. and then cooled to room temperature. The contents were further cooled to 10° C. and maintained for 1 hour at 10° C. The solid obtained was collected by filtration and dried to obtain 3 gm of nilotinib hydrochloride crystalline form H1.

Workup

  1. temperaturecooled to room temperature
  2. temperatureThe contents were further cooled to 10° C.
  3. temperaturemaintained for 1 hour at 10° C
  4. customThe solid obtained
  5. filtrationwas collected by filtration
  6. customdried

Sources & evidence

ORD record
ord-efe445d4e1574c669e1d2c551b6d75de
Source dataset
uspto-grants-2014_04
Patent number
US08703788B2

Reaction notes

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