反应详情

To 200 ml of a solution of 20.0 g potassium carbonate in 250 ml water, 15 g of 3-cyanocinnamic acid was added; the resulting mixture was heated until all the acid was in solution. The solution was cooled and filtered and rinsed with water to 250 ml total volume. Then 0.95 g of 10% palladium on carbon was added and the solution was hydrogenated at 8.5 psi for two hours. The reaction mixture was filtered, and then acidified to a pH of about 1 by the dropwise addition of concentrated hydrochloric acid, being careful to avoid too much foaming. The mixture was chilled in an ice bath and filtered to collect the precipitated product acid. The precipitate was rinsed several times with cold water and dried overnight, to give 13 g of the above-identified product as a solid, melting point 95° C.

1. temperaturethe resulting mixture was heated until all the acid
2. temperatureThe solution was cooled
3. filtrationfiltered
4. washrinsed with water to 250 ml total volume
5. additionThen 0.95 g of 10% palladium on carbon was added
6. filtrationThe reaction mixture was filtered
7. additionacidified to a pH of about 1 by the dropwise addition of concentrated hydrochloric acid
8. temperatureThe mixture was chilled in an ice bath
9. filtrationfiltered
10. customto collect the precipitated product acid
11. washThe precipitate was rinsed several times with cold water
12. customdried overnight