HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 1-Diazo-3-(3,4-dichlorophenyl)-5-(4-hydroxy-4-phenyl-1-piperidinyl)-2-pentanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 5-Bromo-1-diazo-3-(3,4-dichlorophenyl)-2-pentanone | HCID 53781276 | — |
| Produkt | 1-Diazo-3-(3,4-dichlorophenyl)-5-(4-hydroxy-4-phenyl-1-piperidinyl)-2-pentanone | HCID 53915725 | — |
Reaktionsschritte
Dissolve the product of Step 4 (3.93 g, 11.7 mmoles) in 50 ml of dry EtOAc. Add 4-hydroxy-4-phenyl-1-piperidine (2.55 g, 14.4 mmoles), followed by dry Et3N (13.3 ml.). Heat under N2 at 60°-65° C. for 28 h. Cool to room temperature, filter the solid and wash with EtOAc. Apply the filtrate 1 5 to a silica gel column and elute the column with 1.5% CH3OH(NH3)/EtOAc. Yield: 2.34 g; Cl-MS: m/e=432 (M+H+, 35Cl+37Cl isotope).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05840725 |
| Quelldatensatz | uspto-grants-1998_11 |
| ORD ID | ord-6487fd7f66324a05b5df4c52a043a36b |
| Quellennotiz | uspto-grants-1998_11 |