HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-Aminothiophene-3-carboxamide → 2-sulfanyl-3H,4H-thieno(2,3-d)pyrimidin-4-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-Aminothiophene-3-carboxamide | HCID 699495 | — |
| Edukt | Potassium ethylxanthate | HCID 2735045 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-sulfanyl-3H,4H-thieno(2,3-d)pyrimidin-4-one | HCID 3603393 | 69,5% |
Reaktionsbedingungen
| Temperatur | 150 °C |
|---|
Reaktionsschritte
2-Amino-thiophene-3-carboxlic acid amide (28.4 g, 0.2 mol) and potassium ethylxanthate (96 g, 3 eq) were mixed together and added to DMF (1000 mL). The resulting mixture was heated to 150° C. for about six hours. The solvent (DMF) was removed on the rotovap under high vacuum at 90° C. The residue was diluted with 600 mL of aqueous citric acid (5%) and cooled to 0° C. and stirred for about 30 minutes. The tan powder was filtered and dried overnight to give 25.6 g of the title compound ((M+H)+=185, M.P.>300° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07091347B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-9a87187d185b4d9390fcb9daeac9bc76 |
| Quellennotiz | uspto-grants-2006_08 |