Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-{8-(2,6-difluorophenyl)-2-[(1H-imidazol-2-ylmethyl)amino]-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl}-4-methyl-N-1,3-thiazol-2-ylbenzamide | HCID 11948180 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86631881 | HCID 86631881 | 58.1% |
Reaction Steps
Acetone (250 uL) was added to amorphous free-base version of 3-{8-(2,6-difluorophenyl)-2-[(1H-imidazol-2-ylmethyl)amino]-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl}-4-methyl-N-1,3-thiazol-2-ylbenzamide from Example 79c (12.3 mg), and the resulting mixture was heated to about 50° C. Hydrochloric acid was added (1.0 equivalent; 1N in 1,4 dioxane). The mixture was cooled to room temperature and shook for several hours. The product was filtered, washed with acetone, and dried for several hours in a vacuum oven at 50° C. with a slow nitrogen bleed. The yield was 58.1% (7.6 mg) of title compound (melt begins at <50° C. by DSC).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08354416B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-968d450ae6a840d6b325017bd6d4243b |
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| Source note | uspto-grants-2013_01 |
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