HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfolane → 2-Fluoro-5-nitropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfolane | HCID 31347 | — |
| Reactant | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | 2-Fluoro-5-nitropyridine | HCID 95264 | — |
Reaction Steps
A mixture of 5-nitro-2-chloropyridine (2.0 g, 12.6 mmol) and anhydrous potassium fluoride (2.2 g, 38 mmol) in a combination of sulfalone (6 mL) and benzene (4 mL) was stirred at RT for 20 min. The benzene was then removed by distillation. The resulting mixture was heated at 150° C. for 12 h. The mixture was cooled to RT whereupon water (60 mL) was added. The desired product was separated from the solution via steam distillation. Extraction of the distillate with diethyl ether (2×10 mL) followed by drying (Na2SO4) and concentration gave 5-nitro-2-fluoropyridine as a water white oil (1.3 g, 73%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06605725B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-949b3abdd77d4b8396530941a4ae092d |
| Source note | uspto-grants-2003_08 |