HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-Cyano-6-fluoro-3-nitropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | 6-Chloro-3-nitropyridine-2-carbonitrile | HCID 13381705 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 2-Cyano-6-fluoro-3-nitropyridine | HCID 10844807 | — |
Reaction Steps
A mixture of 6-chloro-2-cyano-3-nitropyridine [Colbry, N. L.; Elslager, E. F. ; Werbel, L. M.; J. Het. Chem., 1984, 21, 1521-1525] (10.0 g, 0.054 mol) and KF (9.48 g, 0.163 mol) in MeCN (200 mL) is heated under reflux with stirring for 18 h, then poured into water and extracted with EtOAc. The extract is washed with water and worked up, and the residue is chromatographed on silica gel, eluting with EtOAc/petroleum ether (3:7), to give after removal of the solvent under reduced pressure 2-cyano-6-fluoro-3-nitropyridine (7.2 g, 79%). 1H NMR (CDCl3) δ 8.79 (1H, dd, J=9.0, 6.0 Hz), 7.48 (1H, dd, J=9.0, 3.0 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06084095 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-cc3f09c2f84545549451cf27816d373c |
| Source note | uspto-grants-2000_07 |