HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 2-pyridinecarboxylate → 2-phenyl-1-(pyridin-2-yl)ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 2-pyridinecarboxylate | HCID 17307 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 178418336 | HCID 178418336 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-phenyl-1-(pyridin-2-yl)ethanone | HCID 256073 | 53.6% |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
A solution of ethyl picolinate (1.0 g, 6.62 mmol) in anhydrous tetrahydrofuran (15 mL) was added benzylmagnesium chloride (3.64 mL, 7.28 mmol) at −78° C. The mixture was stirred at −78° C. for 5 h, and poured into saturated aqueous ammonium chloride solution (70 mL), and extracted with ethyl acetate (50 mL×2). The organic layer was washed with brine (80 mL), and dried over anhydrous sodium sulfate. The solvent was removed, and the residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=10:1) to give Intermediate 27 (700 mg, yield 53.6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067893B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-2c512a9121404efbb1e2f886cf94125f |
| Source note | uspto-grants-2015_06 |