Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2-Aminopyridine | HCID 10439 | — |
| Reactant | 8-Cyclopentyl-2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one | HCID 10826395 | — |
| Product | HCID 5330261 | HCID 5330261 | 7% |
Reaction Steps
8-Cyclopentyl-2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one (200 mg, 0.7 mmol) prepared as in Example 107 of WO 98/33798 (incorporated herein by reference) and 2-aminopyridine (130 mg, 1.4 mmol) were combined in a 10 mL round-bottomed flask. The flask was purged with nitrogen (10 min), then heated in a 160° C. oil bath (30 min). After cooling, the orange residue was triturated with water to afford an orange solid, which was further purified by reversed-phase HPLC purification. [Vydac C18 TP254 (30 mm×100 mm); A: ACN (acetonitrile)+0.1% TFA (trifluor acetic acid); B; H2O+0.1% TFA; 10%-76% B over 40 min]. 15 mg of 8-cyclopentyl-2-(pyridin-2-ylamino)-8H-pyrido[2,3-d]pyrimidin-7-one was isolated as a yellow solid. Mp: >250° C., Anal. HPLC [Vydac C18 TP254 (4.6×150 mm); A: ACN+0.1% TFA; B; H2O+0.1% TFA; 10%-76% B over 20 min]: >98% Rt=13.9 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07456168B2 |
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| Source dataset | uspto-grants-2008_11 |
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| ORD ID | ord-67361cb5dec74cf1a8de522519baa41e |
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| Source note | uspto-grants-2008_11 |
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