HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuryl chloride → Ethyl 3-chloro-2-oxopiperidine-3-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuryl chloride | HCID 24648 | — |
| Edukt | 3-Carbethoxy-2-piperidone | HCID 97773 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Ethyl 3-chloro-2-oxopiperidine-3-carboxylate | HCID 568505 | — |
Reaktionsschritte
To a mixture of ethyl 2-oxopiperidine-3-carboxylate (30 g) in THF (300 mL) was added dropwise sulfuryl chloride (14.2 mL) at 0° C-5° C., and the mixture was stirred at room temperature for 18 hr. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution (300 mL) at 0° C., and the mixture was stirred at room temperature for 30 min and extracted with ethyl acetate (300 mL×3). The extract was washed with saturated brine (300 mL), and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was washed with hexane/ethyl acetate (5/1, 60 mL×2) to give the title compound (32.7 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08901309B2 |
| Quelldatensatz | uspto-grants-2014_12 |
| ORD ID | ord-96a2a23957d64f3d8ae5c1875c7c0dd2 |
| Quellennotiz | uspto-grants-2014_12 |