Hydrochloric Acid → Nilotinib Hydrochloride Anhydrous

HRID 1516306Notes

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]>CCO>[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

Conditions

Temperature: 25 °C

Procedure

Nilotinib base form A (0.5 g, 0.94 mmol) was suspended in ethanol absolute (4 ml), then an 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 ethanol absolute (1.5 ml). The solid was dried under vacuum oven at 50° C. overnight to yield Nilotinib HCl form T2.

Workup

filtrationThe product was filtered
washwashed twice with ethanol absolute (1.5 ml)
customThe solid was dried under vacuum oven at 50° C. overnight

Sources & evidence

ORD record: ord-e4e20782f65042d9b5197cbf0934d724
Source dataset: uspto-grants-2012_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08227477B2

Reaction notes

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