تفاعل #1914813

معادلة التفاعل

isopentyl nitrite

HCl

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

isopentyl nitrite

→

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

المردود 81.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىto return to ambient temperature
2. 2
   درجة الحرارةthe reaction mixture was cooled to 5° C.
3. 3
   ترشيحfiltered
4. 4
   غسيلThe solid was washed with absolute MeOH (10 ml)
5. 5
   أخرىwas then triturated twice from heptane
6. 6
   أخرىThe solid was dried under vacuum at 35° C.

الإجراء التجريبي

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.

المصدر