Sulfolane → 2-Fluoro-5-nitropyridine

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%).

1. customThe benzene was then removed by distillation
2. temperatureThe resulting mixture was heated at 150° C. for 12 h
3. temperatureThe mixture was cooled to RT whereupon water (60 mL)
4. additionwas added
5. customThe desired product was separated from the solution via steam distillation
6. extractionExtraction of the distillate with diethyl ether (2×10 mL)
7. customby drying
8. concentration(Na2SO4) and concentration

ORD-Eintrag

ord-949b3abdd77d4b8396530941a4ae092d

Quelldatensatz

uspto-grants-2003_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06605725B2