HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-methyl-2-pyrrolidone → 2-Cyano-5-fluoropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | 5-Chloro-2-cyanopyridine | HCID 3833942 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 2-Cyano-5-fluoropyridine | HCID 11332453 | 56.6% |
Reaction Steps
Add 5-chloro-pyridine-2-carbonitrile (3.0 g, 21.7 mmol) and potassium fluoride (3.9 g, 67.1 mmol) to a flask containing NMP (75 mL). Heat the mixture to reflux for 16 h. Add additional potassium fluoride (1.0 g, 17.2 mmol) and NMP (10 mL), then continue heating at reflux for 3 h. Cool the mixture, dilute with EtOAc, then wash with saturated NaCl (3×50 mL). Collect the organic layer, concentrate in vacuo and purify by chromatography on silica gel eluting with hexane/EtOAc (20:1) to obtain the desired intermediate (1.5 g, 53%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022062B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-a95b1deea9704c119e2dd95556907e84 |
| Source note | uspto-grants-2011_09 |