HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Ethoxy-3-oxo-2-phenylpropanoic acid → HCID 178517418, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Ethoxy-3-oxo-2-phenylpropanoic acid | HCID 2729903 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Edukt | 4-Bromobenzene-1-carboximidamide--hydrogen chloride (1/1) | HCID 12207714 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 178517418 | HCID 178517418 | — |
Reaktionsbedingungen
| Temperatur | 80 °C |
|---|
Reaktionsschritte
Into a solution of 3.45 g (150 mmol) of sodium in 100 ml methanol, here were sequentially added 10.98 g (47 mmol) 4-bromobenzamidine hydrochloride and 11.15 g (47 mmol) of phenyl malonic acid ethyl ester. The mixture was heated for 12 hours at 80° C. The deep yellow reaction solution was filtered to remove the precipitated sodium chloride and thereafter the pyrimidine was precipitated with 10 ml of 2 molar hydrochloric acid as an intensive yellow solid. The solid was sequentially washed with water, ethanol and diethyl ether. Yield: 12.70 g (37 mmol, 79% theory) of yellow solid. The pyrimidine is insoluble in all tested organic solvents as well as in water. m.p. greater >230° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06326327B1 |
| Quelldatensatz | uspto-grants-2001_12 |
| ORD ID | ord-450dc10b50984b4aa5ddbde196c4908c |
| Quellennotiz | uspto-grants-2001_12 |