反应详情

18.3 grams of 3,4,5-trimethoxyaniline and 31.2 g of bis(β-bromoethyl)amine monohydrobromide are mixed with 170 ml of methanol and refluxed by heating under a nitrogen gas stream for 10 hours. After cooling the reaction mixture, 5.3 g of anhydrous sodium carbonate are added to the mixture and refluxed by heating for additional 10 hours. Under reduced pressure, about 70 ml of methanol are removed off by distillation, and the mixture is allowed to staand to cool at room temperature. The crystals thus precipitated are collected by filtration and washed with a small amount of ethanol. Recrystallization from ethanol obtains 38 g of 4-(3,4,5-trimethoxyphenyl)piperazine monohydrobromide in the form of colorless plate-like crystals with a melting point of 227°-228° C.

1. temperaturerefluxed
2. temperatureby heating under a nitrogen gas stream for 10 hours
3. additionare added to the mixture
4. temperaturerefluxed
5. temperatureby heating for additional 10 hours
6. customUnder reduced pressure, about 70 ml of methanol are removed off by distillation
7. customThe crystals thus precipitated
8. filtrationare collected by filtration
9. washwashed with a small amount of ethanol
10. customRecrystallization from ethanol