HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4,5-Dihydro-4-[3-(1-tert-butoxycarbonylpiperidin-4-yl)propan-1-yl]-3H-1,4,8b-triazaacenaphthylen-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | tert-Butyl 4-(3-aminopropyl)piperidine-1-carboxylate | HCID 22990164 | — |
| Reactant | 3-Carbethoxy-5-chloromethylimidazo[1,2-a]pyridine sulfate | HCID 70211102 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4,5-Dihydro-4-[3-(1-tert-butoxycarbonylpiperidin-4-yl)propan-1-yl]-3H-1,4,8b-triazaacenaphthylen-3-one | HCID 21190210 | 62.1% |
Reaction Steps
A solution prepared by dissolving 3.59 g (10.66 mM) of 3-carbethoxy-5-chloromethylimidazo[1,2-a]pyridine sulfate, 3.10 g (12.79 mM) of 3-(1-tert-butoxycarbonylpiperidin-4-yl)-1-propylamine, and 5.94 ml (42.64 mM) of triethylamine in 30 ml of ethanol was refluxed for 5 hours. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was extracted with 100 ml of chloroform. The organic layer was washed with 100 ml of saturated aqueous NaCl solution and dried over MgSO4 and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform-methanol=50:1) to provide 2.55 g (yield 62.1%) of the title compound as yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06251905B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-64254b812252404dbeba8050f6c8f2f1 |
| Source note | uspto-grants-2001_06 |