반응 #1914813

반응 방정식

isopentyl nitrite

HCl

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

isopentyl nitrite

→

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

수율 81.0%

용매

ethanol

반응 조건

후처리

1. 1
   기타to return to ambient temperature
2. 2
   온도the reaction mixture was cooled to 5° C.
3. 3
   여과filtered
4. 4
   세척The solid was washed with absolute MeOH (10 ml)
5. 5
   기타was then triturated twice from heptane
6. 6
   기타The solid was dried under vacuum at 35° C.

실험 절차

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.

출처