HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl p-tolylacetate → 5-(4-Methyl-benzyl)-3-(1-methyl-4-phenyl-butyl)-3,6-dihydro-[1,2,3]triazolo[4,5-d]pyrirnidin-7-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl p-tolylacetate | HCID 90265 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Edukt | HCID 11149992 | HCID 11149992 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 5-(4-Methyl-benzyl)-3-(1-methyl-4-phenyl-butyl)-3,6-dihydro-[1,2,3]triazolo[4,5-d]pyrirnidin-7-one | HCID 135484611 | 57,9% |
Reaktionsschritte
1.0 g (3.8 mmol) of 5-amino-1-(1-methyl-4-phenyl-butyl)-1H-[1,2,3]triazole-4-carboxamide are dissolved in a solution of 439 mg of sodium (19 mmol) in 38 ml of ethanol. 2.22 g (14.6 mmol) of methyl 4-methylphenylacetate are added, and the mixture is then refluxed overnight. The solvent is removed under reduced pressure, the residue is taken up with CH2Cl2, the organic phase is extracted twice with 1N HCl and dried over Na2SO4 and the solvent is removed under reduced pressure. Two chromatographic purifications (cyclohexane/ethyl acetate=3:1) give 853 mg (57%) of a solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06458796B1 |
| Quelldatensatz | uspto-grants-2002_10 |
| ORD ID | ord-1460cf51abcd4fcea40d48200be58237 |
| Quellennotiz | uspto-grants-2002_10 |