HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 69719582, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 22380627 | HCID 22380627 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69719582 | HCID 69719582 | 51% |
Reaction Steps
Subsequently, the resulting 4-aminomethyl-1-(ethoxycarbonyl)-4-(2-methylphenyl)piperidine was dissolved in dichloromethane (10 ml), added with ethyl chloroformate (0.18 ml) and triethylamine (0.26 ml) and stirred at room temperature for 30 minutes. After the reaction mixture was added with water (10 ml) and the layers were separated, the aqueous layer was further extracted with dichloromethane (10 ml). The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: hexane:ethyl acetate=2:1) to obtain 372 mg of the title compound. Yield: 51% (for the two steps).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06916822B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-f56880bc0930403aa813e86cb57f4c99 |
| Source note | uspto-grants-2005_07 |