HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 1-Benzyloxycarbonyl-4-[methoxycarbonyl(ethylamino)]-piperidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Iodoethane | HCID 6340 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Benzyl 4-(methoxycarbonylamino)piperidine-1-carboxylate | HCID 18677680 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 1-Benzyloxycarbonyl-4-[methoxycarbonyl(ethylamino)]-piperidine | HCID 18677725 | 97% |
Reaktionsschritte
To 82 mg (0.28 mmol) of 1-benzyloxycarbonyl-4-(methoxycarbonylamino)piperidine from Step A and 0.045 mL (0.56 mmol) of ethyl iodide in 4 mL of DMF under nitrogen was added 22 mg (0.56 mmol) of 60% sodium hydride in mineral oil. The reaction was stirred at rt for 1 h and was then poured into water containing 1 mL of 2 N hydrochloric acid and extracted twice with ether. The organic layers were each washed with a portion of brine, dried over sodium sulfate, combined and concentrated. The residue was purified by FC eluting with 50% ethyl acetate in hexanes to afford 87 mg of title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06472410B1 |
| Quelldatensatz | uspto-grants-2002_10 |
| ORD ID | ord-db214a4b864645a8968948348e8bc713 |
| Quellennotiz | uspto-grants-2002_10 |