HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanesulfonamide → HCID 66667421, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanesulfonamide | HCID 72879 | — |
| Edukt | 2-Methoxy-4-methylbenzoic acid | HCID 597164 | — |
| Edukt | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Katalysator | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 66667421 | HCID 66667421 | 63% |
Reaktionsschritte
2-Methoxy-4-methyl-benzoic acid (1.0 g. 6 mmol), methanesulphonamide (1.14 g. 12 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.31 g. 12 mmol), 4-dimethylaminopyridine (1.47 g. 12 mmol) and DCM (50 mL) were combined and stirred at room temperature under nitrogen for 18 hours. The reaction mixture was concentrated in vacuo and the residue suspended in water and acidified with aqueous potassium hydrogen sulphate (0.5 M). The mixture was extracted with EtOAc (1×30 mL). The organic layer was separated, washed with brine (2×20 mL), dried over sodium sulfate, filtered and evaporated to give a solid, which was triturated with hexane: diethyl ether (4:1) to yield the title compound as a white solid (0.92 g, 63%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09102621B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-a69f904eb1cb40979a7554961011bfd3 |
| Quellennotiz | uspto-grants-2015_08 |