HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cyclopropylmethylsulphinic acid → 2-Cyclopropylmethanesulfonylmethyl-4-morpholin-4-yl-4-oxo-butyric acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cyclopropylmethylsulphinic acid | HCID 17937320 | — |
| Edukt | 2-Methylene4-morpholin-4-yl-4-oxo-butyric acid | HCID 22054022 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 2-Cyclopropylmethanesulfonylmethyl-4-morpholin-4-yl-4-oxo-butyric acid | HCID 22054098 | 40,1% |
Reaktionsbedingungen
| Temperatur | 85 °C |
|---|
Reaktionsschritte
To a solution of cyclopropylmethylsulphinic acid (1.8 g, 15 mmol) in anhydrous toluene (45 mL) and anhydrous acetonitrile (9 mL) was added 2-Methylene4-morpholin-4-yl-4-oxo-butyric acid (2.98 g, 15 mmol). The resulting solution was warmed to 85° C. and stirred at this temperature for 4.5 h. The heterogeneous reaction mixture is then allowed to cool to room temperature then concentrated under reduced pressure. The residue is then purified by flash chromatography eluting with 7% methanol in dichloromethane to give 2-Cyclopropylmethanesulfonylmethyl-4-morpholin-4-yl-4-oxo-butyric acid (1.92 g) as viscous oil which was re crystallized from hot ethyl acetate to give a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07030116B2 |
| Quelldatensatz | uspto-grants-2006_04 |
| ORD ID | ord-eeb3f2e7ab404a5f96dc1a8bc5ff6cc1 |
| Quellennotiz | uspto-grants-2006_04 |