反应详情

A mixture of 12.3 g. (55 mmole) n-butyl 3-(4-aminophenyl)-propionate, 16.0 g. (55 mmole) N,N-bis-(2-chloroethyl)-4-chloroaniline and 50 ml. n-butanol is maintained at reflux temperature for 48 hours, then 3.8 g. (27 mmole) pulverised anhydrous potassium carbonate are added thereto and stirring continued for 1 week at reflux temperature. Thereafter, it is suction filtered hot, the filtrate is evaporated in a vacuum and the residue is stirred with ligroin and suction filtered. The product is now taken up in diethyl ether, filtered and mixed with hydrogen chloride-containing diethyl ether. Since the hydrochloride is difficult to suction filter, the ether phase is evaporated in a vacuum and the residue recrystallised from n-butanol. Yield 9.5 g. (39% of theory) of hydrochloride; m.p. 179°-183° C. (decomp.).

1. additionA mixture of 12.3 g
2. temperatureat reflux temperature for 48 hours
3. additionare added
4. waitcontinued for 1 week
5. temperatureat reflux temperature
6. filtrationfiltered hot
7. customthe filtrate is evaporated in a vacuum
8. stirringthe residue is stirred with ligroin and suction
9. filtrationfiltered
10. filtrationfiltered
11. additionmixed with hydrogen chloride-
12. additioncontaining diethyl ether
13. filtrationto suction filter
14. customthe ether phase is evaporated in a vacuum
15. customthe residue recrystallised from n-butanol