HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → methyl {(3S)-1-[5-(adamantan-1-ylcarbamoyl)-6-(propylthio)pyridin-2-yl]piperidin-3-yl}acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | methyl 2-[(3S)-piperidin-3-yl]acetate | HCID 40153895 | — |
| Reactant | N-adamantan-1-yl-6-chloro-2-(propylthio)nicotinamide | HCID 59830706 | — |
| Solvent | Butyronitrile | HCID 8008 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | methyl {(3S)-1-[5-(adamantan-1-ylcarbamoyl)-6-(propylthio)pyridin-2-yl]piperidin-3-yl}acetate | HCID 59830770 | 44% |
Reaction Steps
N-adamantan-1-yl-6-chloro-2-(propylthio)nicotinamide (0.365 g, 1 mmol) was added to (S)-methyl 2-(piperidin-3-yl)acetate.HCl (0.194 g, 1 mmol) and potassium carbonate (0.415 g, 3 mmol) in butyronitrile (4 mL) was heated at 150° C. for 2 hours. The reaction mixture was diluted with EtOAc (50 mL), and washed sequentially with water (20 mL) and brine (20 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 50% EtOAc in hexane. Pure fractions were evaporated to dryness to afford methyl {(3S)-1-[5-(adamantan-1-ylcarbamoyl)-6-(propylthio)pyridin-2-yl]piperidin-3-yl}acetate (0.215 g, 44%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07964618B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-80e4e4eb1cc34be293daeb5729fa15b2 |
| Source note | uspto-grants-2011_06 |