HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → HCID 178515060, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-(Chloromethyl)-2,3-dihydro-1lambda6,2-benzothiazole-1,1,3-trione | HCID 2302435 | — |
| Edukt | HCID 178527987 | HCID 178527987 | — |
| Lösungsmittel | Methyl Ethyl Ketone | HCID 6569 | — |
| Produkt | HCID 178515060 | HCID 178515060 | 81,7% |
Reaktionsschritte
A mixture of 2-(chloromethyl) saccharin (3 g, 12.9 mmol) , 1-cyclohexyl-5-mercapto-1H-tetrazole (2.37 g, 12.9 mmol) and potassium carbonate (4.45 g, 32.2 mmol) was heated under reflux in methyl ethyl ketone (50 ml) for 1 hour. The reaction mixture was cooled, poured into dilute sodium bicarbonate/ice solution and extracted twice with ethyl acetate. The combined organic extracts were washed with water, dried (Na2SO4) and freed of solvent under vacuum. Chromatography (silica gel; MDC) afforded 2 g of 2-(1-cyclohexyl-1H-tetrazol-5-ylthiomethyl) saccharin as a white foam that was crystallized from hot cyclohexane, mp 103°-105° C. 1H nmr (90 MHz, CDCl3):5.65 (2H, s). FDMS: m/e 379 (M+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05650422 |
| Quelldatensatz | uspto-grants-1997_07 |
| ORD ID | ord-8cbd179f41b64431aff323ddef88b0d0 |
| Quellennotiz | uspto-grants-1997_07 |