Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Nilotinib | HCID 644241 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 1353151-22-0 | HCID 56592675 | — |
Reaction Steps
A mixture of Nilotinib base (2.00 g, 3.77 mmol) and TFE (12 mL, 6V) was stirred and heated to 55° C. to provide a clear pale yellow solution. The solution was cooled to 50° C. and HBr (48% aq, 0.4 mL, 8.31 mmol, 2.2 eq) was added. The resulting deep yellow solution was stirred at 50° C. for 1 h, and then cooled to ambient temperature. Stirring was continued for 2 h and then the mixture was cooled to 5° C. in an ice-bath. About ⅔V of the solvent were removed under reduced pressure and the resulting mixture was kept in a refrigerator (5° C.) overnight. A solid precipitated and was separated by filtration to give Nilotinib HBr form III.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08937082B2 |
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| Source dataset | uspto-grants-2015_01 |
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| ORD ID | ord-7e132a4ea6054ca8a8b9389126c30e14 |
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| Source note | uspto-grants-2015_01 |
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