Reacción #163110

Ecuación de reacción

2,3,6-trifluoropyridine

HNO3

H2SO4

→

title compound

Rendimiento 50.5%

2,3,6-Trifluoro-5-nitropyridine

Rendimiento 50.5%

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe internal temperature below 40° C
2. 2
   workup.ADDITIONUpon completion of the addition
3. 3
   Temperaturacooled to 0° C
4. 4
   Extracciónthe reaction was extracted with hexanes (2×300 ml)
5. 5
   SecadoThe combined organic fractions were dried over Na2SO4
6. 6
   Filtraciónfiltered
7. 7
   Concentraciónconcentrated

Procedimiento

To neat 2,3,6-trifluoropyridine (12.0 g, 90 mmol) was slowly added fuming HNO3 (142 g, 2254 mmol) and H2SO4 (133 g, 1353 mmol) slow enough to keep the internal temperature below 40° C. Upon completion of the addition, the resulting solution was heated to 60° C. for 30 minutes, and then cooled to 0° C. Ice water (21) was added, and the reaction was extracted with hexanes (2×300 ml) and then DCM (1×300 ml). The combined organic fractions were dried over Na2SO4, filtered, and concentrated to give the title compound (8.1 g, 50%), which was used without further purification.

Fuente