反应详情

An 0.3 g. amount of sodium metal is dissolved in 100 ml. of absolute ethanol, then 7.2 g. of 2-chloro-6-hydrazinopyridine (Example 2) is added, followed by 8.2 g. of 4-chlorocinnamonitrile. The reaction mixture is refluxed for 18 hours, then is evaporated in vacuo to a gum. Water is added to give a solid. The solid is collected and dissolved in dichloromethane, dried over magnesium sulfate and filtered. The filtrate is concentrated while adding hexane to separate yellow crystals on cooling. The product is collected and washed with ether-hexane to give 10.3 g. of tan solid. The solid is dissolved in dichloromethane, filtered through absorbent magnesium silicate, then is concentrated while adding hexane to give the product of the Example as white crystals, m.p. 157°-158°.

1. temperatureThe reaction mixture is refluxed for 18 hours
2. customis evaporated in vacuo to a gum
3. additionWater is added
4. customto give a solid
5. customThe solid is collected
6. dissolutiondissolved in dichloromethane
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. concentrationThe filtrate is concentrated
10. additionwhile adding hexane
11. customto separate yellow crystals
12. temperatureon cooling
13. customThe product is collected
14. washwashed with ether-hexane
15. customto give 10.3 g
16. filtrationfiltered through absorbent magnesium silicate
17. concentrationis concentrated
18. additionwhile adding hexane
19. customto give the product of the Example as white crystals, m.p. 157°-158°