反应详情

A mixture of 250 ml. butan-2-one, 15.47 g. (75 mmole) 1-(4-methoxybenzyl)-piperazine, 19.3 g. (75 mmole) ethyl 4-(2-bromoethyl)-benzoate and 20.7 g. (0.15 mole) powdered potassium carbonate is maintained at reflux temperature for 60 hours, then suction filtered while hot and the filtrate evaporated in a vacuum. After the addition of diethyl ether, the product crystallises, the yield being 17.5 g. (61% of theory) of the desired product; m.p. 75°-76° C. The hydrochloride is precipitated from the filtrate by means of hydrogen chloride-containing diethyl ether. After recrystallisation from aqueous ethanol, there are obtained 7.6 g. (23% of theory) of the desired product; m.p. 280°-281° C.

1. additionA mixture of 250 ml
2. temperatureis maintained
3. temperatureat reflux temperature for 60 hours
4. filtrationsuction filtered while hot and the filtrate
5. customevaporated in a vacuum
6. additionAfter the addition of diethyl ether
7. customthe product crystallises
8. customThe hydrochloride is precipitated from the filtrate by means of hydrogen chloride-
9. additioncontaining diethyl ether
10. customAfter recrystallisation from aqueous ethanol, there
11. customare obtained 7.6 g