HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetonitrile → Benzyl 2-[4-(tert-butoxycarbonylamino)piperidin-1-yl]ethylcarbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | benzyl N-(2-bromoethyl)carbamate | HCID 278694 | — |
| Edukt | 4-(N-Boc-amino)piperidine | HCID 723833 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Benzyl 2-[4-(tert-butoxycarbonylamino)piperidin-1-yl]ethylcarbamate | HCID 22989976 | 93,3% |
Reaktionsschritte
A mixture of phenylmethyl (2-bromoethyl)carbamate (12.9 g, 50 mmol) (prepared from phenylmethyl (2-bromoethyl)carbamate and phenylmethyl chloridocarbonate according to the method of A. J. Brouwer and R. M. J. Liskamp, European Journal of Organic Chemistry (2005), (3), 487-495), 1,1-dimethylethyl 4-piperidinylcarbamate (10 g, 50 mmol), potassium carbonate (6.9 g, 50 mmol), acetonitrile (100 ml) and DMF (30 ml) was heated at 40° C. for 2.5 days. The solvents were decanted from inorganic residues and evaporated. The residue was partitioned between ethyl acetate and dilute brine. The organic extract was dried (MgSO4) and evaporated affording a white solid (17.6 g, 93%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08071592B2 |
| Quelldatensatz | uspto-grants-2011_12 |
| ORD ID | ord-2be4e431668143509c580027eb637861 |
| Quellennotiz | uspto-grants-2011_12 |