Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Ethanesulfonic acid | HCID 11668 | — |
| 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 | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86631882 | HCID 86631882 | 70.6% |
Reaction Steps
Acetone (200 uL) was added to 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 (25.1 mg), and the resulting mixture was heated to 50° C. Ethanesulfonic acid was added (1.0 equivalent; 1N in THF), and the mixture stirred for several days. The product was filtered, washed with acetone, and dried overnight in a vacuum oven at 50° C. with a slow nitrogen bleed. The yield was 70.6% (9.1 mg) of title compound with a melting onset at 296° C. (determined 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-8e5026c9bf924a8e94e32f5f04540f2e |
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| Source note | uspto-grants-2013_01 |
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