HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) → (+/-)-5,8-Dihydro-4-methoxy-7-methyl-5-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-6-carboxylic acid isopropyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) | HCID 2735153 | — |
| Edukt | (+/-)-3,4,5,8-Tetrahydro-7-methyl-5-(3-nitrophenyl)-4-oxo-pyrido[2,3-d]-pyrimidine-6-carboxylic acid isopropyl ester | HCID 136393698 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | (+/-)-5,8-Dihydro-4-methoxy-7-methyl-5-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-6-carboxylic acid isopropyl ester | HCID 13645046 | — |
Reaktionsschritte
Three and 0.7 g (10 mmol) (±)-3,4,5,8-tetrahydro-7-methyl-5-(3-nitrophenyl)-4-oxo-pyrido[2,3-d]-pyrimidine-6-carboxylic acid isopropyl ester and 3.0 g (20 mmol) trimethyloxonium-tetrafluoroborate are stirred in 150 ml 1,2-dichloroethane in nitrogen atmosphere and at room temperature for three hours. The product is extracted twice with 50 ml saturated sodium hydrogen carbonate solution, the organic phase is separated, dried over sodium sulfate and reduced under vacuum. Twice recrystallizing the residue from diisopropyl ether/isopropanol yields the product in the form of colorless crystals with a mp of 212°-213° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04762837 |
| Quelldatensatz | uspto-grants-1988_08 |
| ORD ID | ord-e09c11473fef44f999758252a4e6c990 |
| Quellennotiz | uspto-grants-1988_08 |