Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium | HCID 223 | — |
| Reactant | HCID 59258908 | HCID 59258908 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 59258846 | HCID 59258846 | 54% |
Reaction Steps
To the solution of 8-cyclopentyl-6-(1-(2-(methoxymethoxy)ethyl)-1H-pyrazol-4-yl)-4-methyl-2-(methylsulfonyl)pyrido[2,3-d]pyrimidin-7(8H)-one (80 mg, 0.17 mmol) in 5 ml 1,4-dioxane was babbled through ammonium gas for 10 minutes. The reaction tube was sealed and heated to 100° C. for 30 minutes. The reaction mixture was poured into brine and the precipitate was collected via filtration. The solid was then re-dissolved in 5 ml methanol and a few drop of concentrated HCl was added and the mixture was heated to 50° C. for 5 hours. The reaction mixture was cooled down to room temperature. Solvent was removed via rot vap and the residue was triturated with ethylacetate/hexane to give the title compound (33 mg, 54% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08633204B2 |
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| Source dataset | uspto-grants-2014_01 |
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| ORD ID | ord-fd19188d6f2a4e10b0e36ec410c1eea2 |
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| Source note | uspto-grants-2014_01 |
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