HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | 6-benzyl-3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione | HCID 10016028 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione | HCID 10241423 | 179,8% |
Reaktionsschritte
A solution of 96 g of 6-benzyl-3-methyl-5,6,7,8-tetra-hydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione from c) in 1.5 1 of glacial acetic acid was debenzylated by hydrogenolysis for 6 h on 14.6 g of 10% palladium/activated charcoal at 25° C. and 3.5 bar. After the catalyst had been filtered off, the filtrate was concentrated under reduced pressure. The above preparation was repeated. The two crude products were combined, dissolved in water and precipitated, with stirring, by the addition of 33% sodium hydroxide solution to pH 6.9. The precipitate was washed with water and dried at 60° C. under reduced pressure to give 115.3 g of 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05556854 |
| Quelldatensatz | uspto-grants-1996_09 |
| ORD ID | ord-9554e01e27824ec083075b202565eeed |
| Quellennotiz | uspto-grants-1996_09 |