HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 7-Ethoxy-6-hydroxy-2H-1-benzopyran-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Iodoethane | HCID 6340 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Esculin | HCID 5281417 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 7-Ethoxy-6-hydroxy-2H-1-benzopyran-2-one | HCID 13031686 | — |
Reaktionsschritte
110 g (300 mmol) esculine×1.5 H2O, 70 g (450 mmol) ethyl iodide and 82.8 g (600 mmol) of potassium carbonate are agitated in 400 ml DMF for 30 h at 85° C. This was followed by filtration, reduction of the filtrate to approximately 250 ml, the addition of approximately 200 ml ethanol and crystallization at 0° C. The crystals were boiled in 800 ml of 2N sulfuric acid for 5 h under reflux. The product was vacuum filtered, washed with water and recrystallized from water and ethanol: yield 43.2 g (70%), fusion point 145° to 146° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05428038 |
| Quelldatensatz | uspto-grants-1995_06 |
| ORD ID | ord-fca3f46a3ae048f68d56fb69c68edcef |
| Quellennotiz | uspto-grants-1995_06 |