HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triphenyl phosphite → (S)-methyl 4-ethyl-3-methyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-b]pyrazine-7-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triphenyl phosphite | HCID 7540 | — |
| Edukt | (S)-methyl 6-((1-ethoxy-1-oxopropan-2-yl)(ethyl)amino)-5-nitronicotinate | HCID 58324496 | — |
| Katalysator | Platinum | HCID 23939 | — |
| Katalysator | Ammonium metavanadate | HCID 516859 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | (S)-methyl 4-ethyl-3-methyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-b]pyrazine-7-carboxylate | HCID 59416791 | 57,3% |
Reaktionsschritte
(S)-methyl 6-((1-ethoxy-1-oxopropan-2-yl)(ethyl)amino)-5-nitronicotinate (1.22 g, 3.92 mmol) was dissolved in dichloromethane (12 mL). To this solution were added triphenyl phosphite (5.0 mg, 16 umol), ammonium metavanadate (50.0 mg, 0.427 mmol) and Pt/C (5% wt., 0.200 g). The reaction mixture was hydrogenated at 100 psi at 25° C. for 18 h. The mixture was filtered through a small pad of celite and the pad was washed with dichloromethane (20 mL). The combined filtrates were concentrated in vacuo and crystallized with ethyl ether (50 mL) to afford the title compound as a white solid (0.560 g, 57%). [M+H] calc'd for C12H15N3O3, 250; found, 250.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08822470B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-775ec1dd130c4113987685689fe418f1 |
| Quellennotiz | uspto-grants-2014_09 |