HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 23030621, compound → HCID 57986727, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 23030621 | HCID 23030621 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Solvent | Trifluoroacetic anhydride | HCID 9845 | — |
| Product | HCID 57986727 | HCID 57986727 | 101.5% |
Reaction Steps
To a solution of 1.50 g of 1-(4-ethoxycarbonyl-2-fluorophenyl)piperidine-4-carboxamide in 20 ml of THF, 2.0 ml of triethylamine and 0.9 ml of trifluoroacetic acid anhydride were added at −78° C., and the mixture was stirred at room temperature for 6 hours. The solvent was evaporated, EtOAc was added, and then the organic layer was washed with water and brine, and dried over sodium sulfate. After the evaporation of the solvent, the residue was purified by silica gel column chromatography (eluent: hexane-EtOAc=5:1˜4:1) to obtain 1.43 g of 4-(4-cyanopiperidino)-3-fluorobenzoic acid ethyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07638536B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-30a2a7d74c43467497174dccafac783f |
| Source note | uspto-grants-2009_12 |