反应详情

A mixture of 0.20 g. of sodium metal dissolved in 50 ml. of absolute ethanol, 5.0 g. of 3-chloro-6-hydrazinopyridine and 4.8 g. of crotononitrile is heated at reflux for 18 hours. The procedure of Example 5 is followed through the evaporation of the magnesium silicate filtrate to give a yellow gum. Trituration with hexane gives a yellow solid. The solid is dissolved in dichloromethane. This solution is concentrated by heating on a steam bath while adding hexane, then is cooled in a refrigerator to separate 3.3 g. of the product of the Example as pale yellow crystals, m.p. 168°-170° C.

1. additionA mixture of 0.20 g
2. temperatureat reflux for 18 hours
3. customThe procedure of Example 5 is followed through the evaporation of the magnesium silicate filtrate
4. customto give a yellow gum
5. concentrationThis solution is concentrated
6. temperatureby heating on a steam bath
7. additionwhile adding hexane
8. temperatureis cooled in a refrigerator
9. customto separate 3.3 g