HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Carbon Tetrachloride → Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Carbon Tetrachloride | HCID 5943 | — |
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | tert-Butyl 6-methyl-4-oxo-4,5,6,8-tetrahydropyrido[3,4-d]pyrimidine-7(1H)-carboxylate | HCID 136158782 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate | HCID 59394353 | — |
Reaktionsschritte
A solution of (±)-6-methyl-4-oxo-4,5,6,8-tetrahydro-3H-pyrido[3,4-d]pyrimidine-7-carboxylic acid tert-butyl ester, (7.5 g, 28.3 mmol), triphenylphosphine (14.8 g, 56.5 mmol) and carbon tetrachloride (8.2 mL, 85 mmol) in 1,2-DCE (100 mL) is heated at 80° C. for 6 h. At that time the solution is concentrated in vacuo and the residue is separated via FCC (5-60% EtOAc/heptane) to give the title compound. MS (ESI) m/z 284.1 (M+H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08541432B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-9e9734a2181b49b18187f5c64442815c |
| Quellennotiz | uspto-grants-2013_09 |