HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → HCID 178418772, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Acetamidine monohydrochloride | HCID 67170 | — |
| Edukt | Ethyl 3-(4-Fluorophenyl)-3-Oxopropanoate | HCID 2758844 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 178418772 | HCID 178418772 | 87,6% |
Reaktionsschritte
8.7 kg of ethyl 3-(4-fluorophenyl)-3-oxopropionate, 11.7 kg of acetoamidine hydrochloride and 28.6 kg of potassium carbonate were stirred for 5 hours at about 50° C. in 34.5 kg of methanol. Insolubles were separated from the reaction mixture and washed with methanol, and the mother liquor and the washing were combined with water and neutralized with an 18% aqueous solution of hydrochloric acid. After neutralization, the crystal was ripened by stirring under reflux for 4 hours, and the precipitated crystal was isolated by centrifugation, washed with water, dried to obtain 7.4 kg of the target compound as a white crystal.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07091206B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-87d3e58ebd044febb2246a63639c98ea |
| Quellennotiz | uspto-grants-2006_08 |