Reacción #1914813

Ecuación de reacción

isopentyl nitrite

HCl

2-pyridin-2-yl-2H-pyrazol-3-ylamine

isopentyl nitrite

→

4-nitroso-2-pyridin-2-yl-2H-pyrazol-3-ylamine

Rendimiento 81.0%

Disolventes

ethanol

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroto return to ambient temperature
2. 2
   Temperaturathe reaction mixture was cooled to 5° C.
3. 3
   Filtraciónfiltered
4. 4
   LavadoThe solid was washed with absolute MeOH (10 ml)
5. 5
   Otrowas then triturated twice from heptane
6. 6
   OtroThe solid was dried under vacuum at 35° C.

Procedimiento

HCl (37%, 11 μl) was added to a heterogeneous solution of 2-pyridin-2-yl-2H-pyrazol-3-ylamine (2.2 g, 13.7 mmol) in absolute ethanol (15 ml). The reaction mixture was subsequently cooled to 0° C. and isopentyl nitrite (2.02 ml, 15 mmol) was slowly added. The reaction mixture became dark. After the isopentyl nitrite had been completely added, the reaction mixture was allowed to return to ambient temperature. After 2.5 h at ambient temperature, the reaction mixture was cooled to 5° C. and filtered. The solid was washed with absolute MeOH (10 ml) and was then triturated twice from heptane. The solid was dried under vacuum at 35° C. to give 4-nitroso-2-pyridin-2-yl-2H-pyrazol-3-ylamine (2.1 g, 81%) in the form of a green solid.

Fuente