Hydrochloric Acid → Nilotinib Hydrochloride Anhydrous

HRID 1516307Notes

Reaction equation

HRID 1516307 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]>C(O)(C)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]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 644241Nilotinib

Product 1

HCID 16006490Nilotinib Hydrochloride Anhydrous

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Conditions

Temperature
25 °C

Procedure

Nilotinib base form A (0.5 g, 0.94 mmol) was suspended in iso-propanol (4 ml), then HCl solution (0.23 mL, 19.48% in IPA) was added and the reaction mixture became yellow. The slurry was stirred at room temperature (20-30° C.) for 16 h. The product was filtered and washed twice with. iso-propanol (1.5 ml). The solid was dried under vacuum oven at 50° C. overnight to yield Nilotinib HCl form T2.

Workup

  1. filtrationThe product was filtered
  2. washwashed twice with
  3. customThe solid was dried under vacuum oven at 50° C. overnight

Sources & evidence

ORD record
ord-8c2880922cc7491da38f8e32b4fad7ee
Source dataset
uspto-grants-2012_07
Patent number
US08227477B2

Reaction notes

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