HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triphenylphosphine → 4-(1-t-Butoxycarbonylpiperidin-4-yloxy)-3,5-dichloronitrobenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | 2,6-Dichloro-4-nitrophenol | HCID 12066 | — |
| Edukt | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Edukt | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-(1-t-Butoxycarbonylpiperidin-4-yloxy)-3,5-dichloronitrobenzene | HCID 18542604 | 72,2% |
Reaktionsschritte
To a solution of 1-t-butoxycarbonyl-4-hydroxypiperidine (677 mg), 2,6-dichloro-4-nitrophenol (700 mg) and triphenylphosphine (1150 mg) in dichloromethane (40 ml) was added dropwise diethyl azodicarboxylate (0.67 ml) in an ice bath and the mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated in vacuo. The residue was purified by chromatography on a silica gel column using hexane/ethyl acetate=6/1 as an eluant to give the desired compound (950 mg, yield 72%) as a colorless solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06555556B1 |
| Quelldatensatz | uspto-grants-2003_04 |
| ORD ID | ord-58ca57e0caa8443f854973a92ec00d16 |
| Quellennotiz | uspto-grants-2003_04 |