反应 #1914813

反应方程式

isopentyl nitrite

HCl

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

isopentyl nitrite

→

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

收率 81.0%

溶剂

ethanol

反应条件

后处理

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

实验过程

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.

来源