反应详情

A mixture consisting of 9.3 g of 2-trifluoromethylbenzonitrile, 4.5 g of acetonitrile, 4.3 g of sodium amide and 100 ml of ether is stirred and refluxed under nitrogen over night. The resulting solid is collected on a Buchner-funnel, washed with ether and dissolved in approximately 100 ml of cold ethanol. Crushed ice is added to this solution until the total volume is about 700 ml. This mixture is allowed to stand for several hours. The resulting solid precipitate is collected by filtration then dissolved in methanol and decolorizing charcoal is added. The charcoal/methanol mixture is filtered and the filtrate is gradually treated with water until crystallization is judged complete. The crystalline solid is collected and dried under vacuum, to give 7.75 g of β-amino-2-trifluoromethylcinnamonitrile, mp 101°-103°.

1. temperaturerefluxed under nitrogen over night
2. customThe resulting solid is collected on a Buchner-funnel
3. washwashed with ether
4. dissolutiondissolved in approximately 100 ml of cold ethanol
5. additionCrushed ice is added to this solution until the total volume is about 700 ml
6. waitto stand for several hours
7. filtrationThe resulting solid precipitate is collected by filtration
8. dissolutionthen dissolved in methanol
9. additionis added
10. filtrationThe charcoal/methanol mixture is filtered
11. additionthe filtrate is gradually treated with water until crystallization
12. customThe crystalline solid is collected
13. customdried under vacuum