Reaktion #1914813

Reaktionsgleichung

isopentyl nitrite

HCl

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

isopentyl nitrite

→

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

Ausbeute 81.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto return to ambient temperature
2. 2
   Temperaturthe reaction mixture was cooled to 5° C.
3. 3
   Filtrationfiltered
4. 4
   WaschenThe solid was washed with absolute MeOH (10 ml)
5. 5
   Sonstigewas then triturated twice from heptane
6. 6
   SonstigeThe solid was dried under vacuum at 35° C.

Vorschrift

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.

Quelle