反应详情

As for Example 4 a 0.2 g. amount of sodium metal is dissolved in 50 ml. of absolute ethanol, then 5.0 g. of 5-chloro-2-hydrazinopyridine (Example 3) is added, followed by 4.8 g. of methacrylonitrile. The reaction mixture is refluxed for 18 hours. The solvent is removed in vacuo and water is added to give a gum which solidifies. The solid is collected by filtration, and washed with water. The solid is dissolved in dichloromethane, dried over magnesium sulfate and filtered through anhydrous magnesium silicate. The filtrate is evaporated and the residue is triturated with hexane to give a brown solid. The solid is dissolved in dichloromethane and hexane is added while concentrating to separate a solid. The mixture is cooled and filtered to give 3.4 g. of a gray solid. The desired product is recrystallized from dichloromethane-hexane to give a white solid, m.p. 159°-160° C.

1. temperatureThe reaction mixture is refluxed for 18 hours
2. customThe solvent is removed in vacuo and water
3. additionis added
4. customto give a gum which
5. filtrationThe solid is collected by filtration
6. washwashed with water
7. dissolutionThe solid is dissolved in dichloromethane
8. dry with materialdried over magnesium sulfate
9. filtrationfiltered through anhydrous magnesium silicate
10. customThe filtrate is evaporated
11. customthe residue is triturated with hexane
12. customto give a brown solid
13. concentrationwhile concentrating
14. customto separate a solid
15. temperatureThe mixture is cooled
16. filtrationfiltered
17. customto give 3.4 g
18. customThe desired product is recrystallized from dichloromethane-hexane
19. customto give a white solid, m.p. 159°-160° C.