HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Ethoxycarbonyl-5-(pyrazin-2-yl)-1,2-dithiole-3-thione → 4-Carboxy-5-(pyrazin-2-yl)-1,2-dithiole-3-thione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Ethoxycarbonyl-5-(pyrazin-2-yl)-1,2-dithiole-3-thione | HCID 21329210 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 4-Carboxy-5-(pyrazin-2-yl)-1,2-dithiole-3-thione | HCID 21329166 | 72,1% |
Reaktionsbedingungen
| Temperatur | 20 °C |
|---|
Reaktionsschritte
A solution of 4-ethoxycarbonyl-5-(pyrazin-2-yl)-1,2-dithiole-3-thione (150 g) [prepared as described in Example 31] in acetic acid (6750 cc), concentrated sulphuric acid (515 cc) and water (515 cc) is heated for 2 hours under reflux. After cooling, the product which crystallises is filtered off and washed successively with acetic acid (100 cc) and carbon disulphide (2 × 100 cc). This product is then suspended in water (1350 cc) and stirred for 48 hours at a temperature of about 20° C. The insoluble product is then filtered off and washed with water (2 × 250 cc). After drying, 4-carboxy-5-(pyrazin-2-yl)-1,2-dithiole-3-thione (97.5 g), melting at 225° C., is obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04138487 |
| Quelldatensatz | uspto-grants-1979_02 |
| ORD ID | ord-fc7b834283fc4ee5b68660c384723a61 |
| Quellennotiz | uspto-grants-1979_02 |