HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → tert-Butyl 6-methyl-4-oxo-4,5,6,8-tetrahydropyrido[3,4-d]pyrimidine-7(1H)-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Ammonium formate | HCID 2723923 | — |
| Edukt | 6-methyl-7-(1-phenyl-ethyl)-5,6,7,8-tetrahydro-3H-pyrido[3,4-d]pyrimidin-4-one | HCID 136158781 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Produkt | tert-Butyl 6-methyl-4-oxo-4,5,6,8-tetrahydropyrido[3,4-d]pyrimidine-7(1H)-carboxylate | HCID 136158782 | — |
Reaktionsschritte
To a mixture of 6-methyl-7-(1-phenyl-ethyl)-5,6,7,8-tetrahydro-3H-pyrido[3,4-d]pyrimidin-4-one, (6.8 g, 25.2 mmol), ammonium formate (7.96 g, 126 mmol), BOC-anhydride (8.27 g, 37.9 mmol), MeOH (250 mL), and THF (167 mL) is added 10% Pd/C (1.36 g, 20% w/w) and the reaction is heated at reflux for 3 h. The mixture is then filtered through a Celite® pad and the filterate is concentrated. The residue is purified via FCC (1-10% MeOH/DCM) to give the title compound. MS (ESI) m/z 266.1 (M+H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08242125B2 |
| Quelldatensatz | uspto-grants-2012_08 |
| ORD ID | ord-ab7eb85904a142fd9a2e81e119b0cf5d |
| Quellennotiz | uspto-grants-2012_08 |