反应详情

A 2.8 g. amount of sodium metal is dissolved in 200 ml. of absolute ethanol, then 21.35 g. of 3,4-dichlorophenylhydrazine hydrochloride is added followed in 10 minutes by 5.5 g. of acrylonitrile. The reaction mixture is refluxed for 4 hours then most of the ethanol is removed in vacuo. Water is added to separate a solid. The solid is collected by filtration and dried. The solid is dissolved in methanol, treated with activated charcoal and filtered. The filtrate is evaporated to give a solid. The solid is recrystallized from methanol to give the desired product as tan crystals, m.p. 182°-183.5° C.

1. temperatureThe reaction mixture is refluxed for 4 hours
2. custommost of the ethanol is removed in vacuo
3. additionWater is added
4. customto separate a solid
5. filtrationThe solid is collected by filtration
6. customdried
7. dissolutionThe solid is dissolved in methanol
8. additiontreated with activated charcoal
9. filtrationfiltered
10. customThe filtrate is evaporated
11. customto give a solid
12. customThe solid is recrystallized from methanol