HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → Ethyl 3-(3,4-difluorophenyl)-2-thioxopiperidine-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | Ethyl 3-(3,4-difluorophenyl)-2-oxopiperidine-3-carboxylate | HCID 66607999 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Ethyl 3-(3,4-difluorophenyl)-2-thioxopiperidine-3-carboxylate | HCID 86662973 | 116.1% |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
Under an argon atmosphere, Lawesson's reagent (1.00 g) was added to a suspension of ethyl 3-(3,4-difluorophenyl)-2-oxopiperidine-3-carboxylate (1.00 g) in toluene (20 mL) at room temperature. The reaction mixture was stirred at 110° C. for 4 hr, and allowed to cool to room temperature, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane) to give the title compound (859 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822699B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-3c8ee0485f7d48f3af8d7a9297adf0a4 |
| Source note | uspto-grants-2014_09 |