HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl 2-chloroacetoacetate → Ethyl cis(+/-)-2-(4-{[(benzyloxy)carbonyl]amino}-3-methoxypiperidin-1-yl)-4-methyl-1,3-oxazole-5-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl 2-chloroacetoacetate | HCID 11858 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | cis(+/-)-Benzyl (1-carbamoyl-3-methoxypiperidin-4-yl)carbamate | HCID 131730860 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Ethyl cis(+/-)-2-(4-{[(benzyloxy)carbonyl]amino}-3-methoxypiperidin-1-yl)-4-methyl-1,3-oxazole-5-carboxylate | HCID 86648586 | 31,1% |
Reaktionsschritte
cis(±)-Benzyl (1-carbamoyl-3-methoxypiperidin-4-yl)carbamate obtained in Example (103b) (0.92 g, 3 mmol), ethyl α-chloroacetoacetate (3.29 g, 20 mmol) and sodium bicarbonate (0.84 g, 10 mmol) were stirred at 120° C. for three hours. The reaction solution was diluted with ethyl acetate, washed with water and brine, and dried over anhydrous magnesium sulfate. Following concentration under reduced pressure, the residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=1/4, 1/2, 2/1, 4/1) to obtain 0.39 g of the title compound as a light brown solid (27%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08536197B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-30f44b51507f4bd78b3a48bf8acb5563 |
| Quellennotiz | uspto-grants-2013_09 |