反应详情

A mixture of 175 g. (0.79 mole) n-butyl 3-(-4-aminophenyl)-propionate (prepared by the hydrogenation of n-butyl 4-nitrocinnamate in the presence of palladiumcharcoal in n-butanol; b.p. 137°-138° C./0.013 mbar), 141.3 g. (0.79 mole) bis-(2-cholorethyl)-amine hydrochloride and 600 ml. n-butanol is maintained at reflux temperature for 48 hours, then 54.5 g. (0.39 mole) powdered potassium carbonate are added thereto and the reaction allowed to continue for a further 120 hours at the boiling temperature. Thereafter, the reaction mixture is suction filtered hot, the filtrate is evaporated in a vacuum and the oil remaining behind is taken up in n-butanol. The sulphate is now precipitated out in the cold by adding concentrated sulphuric acid. It is filtered off with suction, triturated with diethyl ether and dried. Yield 286.8 g. (69% of theory); m.p. 183°-185° C.

1. additionA mixture of 175 g
2. temperatureat reflux temperature for 48 hours
3. additionare added
4. filtrationfiltered hot
5. customthe filtrate is evaporated in a vacuum
6. customThe sulphate is now precipitated out in the cold
7. additionby adding concentrated sulphuric acid
8. filtrationIt is filtered off with suction
9. customtriturated with diethyl ether
10. customdried