反应详情

5.0 Grams of 6-(1-oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride and 5.0 g of m-chloroaniline were mixed in 30 ml of concentrated hydrochloric acid and the mixture was heated at 200°-220° C. by removing water for 6 hours. After cooled the reaction mixture 100 ml of 5N-hydrochloric acid was added thereto and dissolved by heating and refluxed for 2 hours. Then the reaction mixture was cooled and poured into 100 ml of 8N-sodium hydroxide aqueous solution and the organic layer was extracted with chloroform. Chloroform was removed by distillation and the residue thus obtained was separated and purified by a preparative silica-gel thin layer chromatography, then recrystallized from dioxane-water to obtain 0.16 g of 6-{1-oxo-2-[4-(3-chlorophenyl)-1-piperazinyl]-ethyl}-3,4-dihydrocarbostyril in light yellow needle-like crystals.

1. temperaturethe mixture was heated at 200°-220° C.
2. customby removing water for 6 hours
3. temperatureAfter cooled the reaction mixture 100 ml of 5N-hydrochloric acid
4. additionwas added
5. dissolutiondissolved
6. temperatureby heating
7. temperaturerefluxed for 2 hours
8. temperatureThen the reaction mixture was cooled
9. additionpoured into 100 ml of 8N-sodium hydroxide aqueous solution
10. extractionthe organic layer was extracted with chloroform
11. customChloroform was removed by distillation
12. customthe residue thus obtained
13. customwas separated
14. custompurified by a preparative silica-gel thin layer chromatography
15. customrecrystallized from dioxane-water