HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → Tert-butyl 4-carbamimidoylpiperidine-1-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | HCID 178451986 | HCID 178451986 | — |
| Katalysator | Nickel | HCID 935 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | Tert-butyl 4-carbamimidoylpiperidine-1-carboxylate | HCID 44828660 | 96,9% |
Reaktionsbedingungen
| Temperatur | 50 °C |
|---|
Reaktionsschritte
Into a 2-L round-bottom flask purged and maintained with an inert atmosphere of argon, was placed tert-butyl 4-(N-hydroxycarbamimidoyl)piperidine-1-carboxylate (46.5 g, 181.56 mmol, 1.00 equiv, 95%), methanol (1500 mL), acetic acid (20 mL), and Raney-Ni (13 g). The reaction system was bubbled for 5 times with hydrogen. The resulting mixture was stirred for 3 h at 50° C. in an oil bath. The solids were filtered out. The resulting solution was concentrated under vacuum to afford 40 g of tert-butyl 4-carbamimidoylpiperidine-1-carboxylate as yellow green crude oil, which was used directly for next step without further purification. MS m/z [M+H]+ (ESI): 278.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09221809B2 |
| Quelldatensatz | uspto-grants-2015_12 |
| ORD ID | ord-07e5935378e142639bd1e691f0f835f7 |
| Quellennotiz | uspto-grants-2015_12 |