反应详情

4-Chloropyrimidine hydrochloride (3.5 g) was added to a stirred suspension of 1-benzyl-4-[4-piperidylcarbonyl]piperazine (6.6 g), triethylamine (12.8 ml) and ethanol (120 ml). The mixture was heated under reflux for four hours and evaporated in vacuo to yield a treacle like substance. The residue was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried (Na2SO4) and evaporated. The residue was absorbed onto alumina and purified using dry flash chromatography eluting with increasingly polar mixtures of dichloromethane and methanol (1:0 to 98:2). The material obtained was triturated with diethylether to give 1-(benzyl)-4-[1 -(4-pyrimidinyl)-4-piperidylcarbonyl]piperazine (3.8 g, 45% yield), mp 107-108.5° C.;

1. temperatureThe mixture was heated
2. temperatureunder reflux for four hours
3. customevaporated in vacuo
4. customto yield a treacle like substance
5. customThe residue was partitioned between ethyl acetate and water
6. washThe organic phase was washed with brine
7. dry with materialdried (Na2SO4)
8. customevaporated
9. customThe residue was absorbed onto alumina
10. custompurified
11. customusing dry flash chromatography
12. washeluting
13. temperaturewith increasingly polar mixtures of dichloromethane and methanol (1:0 to 98:2)
14. customThe material obtained
15. customwas triturated with diethylether