HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nicotinoyl chloride → Ethyl 3-oxo-3-(pyridin-3-yl)-2-(thiophen-3-yl)propanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nicotinoyl chloride | HCID 82604 | — |
| Reactant | Ethyl 3-thiopheneacetate | HCID 520865 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 3-oxo-3-(pyridin-3-yl)-2-(thiophen-3-yl)propanoate | HCID 66665073 | 38% |
Reaction Steps
To a solution of ethyl 2-(thiophen-3-yl)acetate (2.3 g, 16.2 mmol) in anhydrous THF (20 mL) was added LiHMDS (19.4 mL, 19.44 mmol) at −78° C. After stirring at that temperature for 0.5 h, a solution of nicotinoyl chloride (2.8 g, 16.2 mmol) in anhydrous THF (10 mL) was added into the reaction mixture and stirred at −78° C. for 4 hours. The mixture was quenched with NH4Cl solution, extracted with EtOAc. The organic layer was concentrated in vacuo and purified by silica gel column chromatography (1.7 g, yield 38%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946434B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-c5582b8a1bf0419d90d3d59898972ce4 |
| Source note | uspto-grants-2015_02 |