反応 #1914813

反応方程式

isopentyl nitrite

HCl

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

isopentyl nitrite

→

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

収率 81.0%

溶媒

ethanol

反応条件

後処理

1. 1
   その他to return to ambient temperature
2. 2
   温度the reaction mixture was cooled to 5° C.
3. 3
   ろ過filtered
4. 4
   洗浄The solid was washed with absolute MeOH (10 ml)
5. 5
   その他was then triturated twice from heptane
6. 6
   その他The solid was dried under vacuum at 35° C.

実験手順

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.

出典