HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → HCID 16782287, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Picolyl chloride hydrochloride | HCID 23392 | — |
| Edukt | 4-Mercaptobenzoic acid | HCID 95738 | — |
| Lösungsmittel | Water ethanol | HCID 19096565 | — |
| Produkt | HCID 16782287 | HCID 16782287 | 40,9% |
Reaktionsschritte
An ethanol/water mixed solution (2/1, 60 mL) of 4-mercaptobenzenecarboxylic acid (1.0 g), 2-chloromethylpyridine hydrochloride (2.1 g) and potassium carbonate (4.5 g) was heated under reflux for 4 hours. The organic solvent was evaporated off under reduced pressure, and aqueous 5 N hydrochloric acid solution was added to the residue until it became acidic. Water was evaporated off under reduced pressure, and DMF was added to the resulting residue and filtered. The filtrate was concentrated under reduced pressure, and the resulting residue was purified through silica gel column chromatography (chloroform/methanol=9/1 to 4/1) to obtain the entitled compound (650 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07566781B2 |
| Quelldatensatz | uspto-grants-2009_07 |
| ORD ID | ord-e616d6cef73c4db7ba90b40ae60674af |
| Quellennotiz | uspto-grants-2009_07 |