反应详情

A solution of 4-cyanobenzoyl chloride (298 mg) in methylene chloride (10 ml) was added to a stirred mixture of 1-[1(4-pyrimidinyl) piperidin-4-ylcarbonyl]piperazine (412.5 mg) and triethylamine (0.28 ml) in methylene chloride (15 ml) and the resultant mixture was stirred at ambient temperature for 2 hours. The mixture was partitioned between methylene chloride and water. The organic phase was washed with water, dried (Na2SO4) and evaporated. The residue was purified by column chromatography using 0.5% methanol in methylene chloride. Recrystallisation from ethyl acetate/hexane gave, as a solid 1-(4-cyanobenzoyl)-4-[1-(4-pyrimidinyl)piperidin-4-ylcarbonyl] piperazine (280 mg): mpt 192-193° C.;

1. customThe mixture was partitioned between methylene chloride and water
2. washThe organic phase was washed with water
3. dry with materialdried (Na2SO4)
4. customevaporated
5. customThe residue was purified by column chromatography
6. customRecrystallisation from ethyl acetate/hexane