HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → tert-Butyl 4-(6-nitro-1H-indazol-1-yl)piperidine-1-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 6-Nitroindazole | HCID 24239 | — |
| Edukt | 1-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine | HCID 4184869 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | tert-Butyl 4-(6-nitro-1H-indazol-1-yl)piperidine-1-carboxylate | HCID 68609514 | 24,6% |
Reaktionsschritte
6-Nitro-1H-indazole (12.26 mmol, 2 g), tert-butyl 4-(methylsulfonyloxy)piperidine-1-carboxylate (12.26 mmol, 3.42 g) and potassium carbonate (24.52 mmol, 3.39 g) were combined and heated to 100° C. in N,N-dimethylformamide (40 mL) for 4 hours. The reaction mixture was diluted with ethyl acetate and washed with water. The organic phase was dried over sodium sulfate and concentrated at reduced pressure. The resulting residue was purified by silica chromatography (eluting with a solvent gradient from 20% ethyl acetate/heptane to 60% ethyl acetate/heptane) to afford the title compound (1.045 g). MS (ESI) m/z 347.2 [M+H]+
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09108939B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-fca53bf4e3b2464b842024cedb7bc183 |
| Quellennotiz | uspto-grants-2015_08 |