反应详情

温度

150 °C

31.6 g of 2-chloro-3-nitro-pyridine and 56.5 g of 2-amino-pyridine were well mixed in a mortar and the mixture was slowly heated on an oil bath to the melting point. At 150° C. a lively reaction started and the temperature spontaneously rose to 160° C. The heating was suspended until the isothermic reaction ceased and heating at 150° C. was continued for 2 hours. The mixture was cooled and the fused mass was taken up in 500 ml of chloroform. The mixture was concentrated and was chromatographed over silica gel. Elution with about 3 liters of a 1-0.75-1.2 chloroform-benzene-ether mixture yielded unreacted 2-chloro-3-nitro-pyridine and evaporation of the eluent yielded 20 g of raw product which was crystallized from 95% ethanol to obtain 15.5 g (36% yield) of 2-(2-pyridylamino)-3-nitro-pyridine in the form of orange-yellow needles melting at 121°-123° C. The product was soluble in 2 N hydrochloric acid.

1. temperaturethe mixture was slowly heated on an oil bath to the melting point
2. customAt 150° C. a lively reaction
3. customspontaneously rose to 160° C
4. customThe heating was suspended until the isothermic reaction
5. temperatureThe mixture was cooled
6. concentrationThe mixture was concentrated
7. customwas chromatographed over silica gel
8. washElution with about 3 liters of a 1-0.75-1.2 chloroform-benzene-ether mixture
9. customyielded unreacted
10. custom2-chloro-3-nitro-pyridine and evaporation of the eluent
11. customyielded 20 g of raw product which
12. customwas crystallized from 95% ethanol