反应详情

A mixture of 25.8 grams of 1-ethoxycarbonyl-cis-3,5-dimethylpiperazine, 38.6 grams of propyl 4-toluenesulfonate, 90 ml. of absolute ethanol and 9.5 grams of sodium carbonate is stirred and heated to reflux. After 30 minutes of reflux, vigorous evolution of carbon dioxide begins and continues for about 5 hours. Refluxing is continued for a total of 22 hours. The reaction mixture is then cooled and filtered and the solvent is evaporated. The resulting residue is mixed with 300 ml. of aqueous 1 N sodium hydroxide solution and the mixture is extracted with ethyl ether. The ether extract is washed successively with 100 ml. of aqueous 1 N sodium hydroxide and 100 ml. of water and then dried over anhydrous sodium sulfate. The organic solution is then treated with charcoal and the solvent is evaporated to leave a residue which is purified by chromatography to give 4-ethoxycarbonyl-cis-2,6-dimethyl-1-propylpiperazine.

1. temperatureheated to reflux
2. temperatureAfter 30 minutes of reflux
3. temperatureRefluxing
4. customis continued for a total of 22 hours
5. temperatureThe reaction mixture is then cooled
6. filtrationfiltered
7. customthe solvent is evaporated
8. additionThe resulting residue is mixed with 300 ml
9. extractionof aqueous 1 N sodium hydroxide solution and the mixture is extracted with ethyl ether
10. extractionThe ether extract
11. washis washed successively with 100 ml
12. dry with materialof water and then dried over anhydrous sodium sulfate
13. additionThe organic solution is then treated with charcoal
14. customthe solvent is evaporated
15. customto leave a residue which
16. customis purified by chromatography