HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 4-Bromo-1,1,1-trifluorobutane | HCID 521006 | — |
| Edukt | 7-Allyl-8-chloro-1H-purine-2,6(3H,7H)-dione | HCID 59299532 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione | HCID 59299588 | 40% |
Reaktionsbedingungen
| Temperatur | 50 °C |
|---|
Reaktionsschritte
A solution of 8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (2.0 g, 8.8 mmol) in DMF (20 ml) was treated with sodium carbonate (1.15 g, 10.8 mmol) and 4-bromo-1,1,1-trifluorobutane (1.86 g, 9.7 mmol). The mixture was stirred at 50° C. for 18 h then cooled and evaporated. The residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The residue was triturated in a mixture of diethyl ether and cyclohexane then the product filtered off and dried to yield the title compound as a white solid (1.18 g, 40%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08143264B2 |
| Quelldatensatz | uspto-grants-2012_03 |
| ORD ID | ord-9da0aabc817a471d9ca88ff34cc418da |
| Quellennotiz | uspto-grants-2012_03 |