反应详情

4-Amino-6,7-dimethoxy-2-(piperazin-1-yl)quinoline (1.26 g) and 2-chloro-4-dimethylaminopyrimidine (0.76 g) in n-butanol (60 ml) were heated under reflux for 16 hours. The mixture was then evaporated in vacuo, the residue partitioned between chloroform and sodium carbonate solution (10%) and the aqueous phase extracted with chloroform. The combined extracts were washed with water, dried (Na2SO4), evaporated in vacuo and the residue chromatographed on silica gel (Merck 9385). Elution with chloroform-methanol (100:0→95.5) followed by treatment of the product with ethereal hydrogen chloride and recrystallisation from methanol gave 4-amino-6,7-dimethoxy-2-[4-(4-dimethylaminopyrimidin-2-yl)piperazin-1-yl]quinoline dihydrochloride dihydrate (0.19 g), m.p. 260°-263°.

1. temperatureunder reflux for 16 hours
2. customThe mixture was then evaporated in vacuo
3. customthe residue partitioned between chloroform and sodium carbonate solution (10%)
4. extractionthe aqueous phase extracted with chloroform
5. washThe combined extracts were washed with water
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customthe residue chromatographed on silica gel (Merck 9385)
9. washElution with chloroform-methanol (100:0→95.5)
10. customfollowed by treatment of the product with ethereal hydrogen chloride and recrystallisation from methanol