HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → Methyl 4-(4-methylpiperazin-1-yl)benzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-Methylpiperazine | HCID 53167 | — |
| Edukt | Methyl 4-fluorobenzoate | HCID 67878 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Methyl 4-(4-methylpiperazin-1-yl)benzoate | HCID 1472668 | — |
Reaktionsschritte
4-Fluorobenzoic acid methyl ester (34 mmol), 1-methyl-piperazine (75 mmol) and potassium carbonate (34 mmol) are suspended in acetonitrile (30 ml) and stirred under reflux for three days. After evaporation of the solvent, the residue is dissolved in water and extracted three times with ethyl acetate. The extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=95:5) as mobile phase. The product containing fractions are combined and evaporated. The residue is suspended in diethylether/pentane and the solid filtered of and dried (vacuum). A pale yellow powder with mp. 117-119° C., Rf=0.20 (CH2Cl2/MeOH=95:5) is obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06642239B2 |
| Quelldatensatz | uspto-grants-2003_11 |
| ORD ID | ord-f8e68535ffe6496eb0ba31d65120bc69 |
| Quellennotiz | uspto-grants-2003_11 |