HRID2305356
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4-Bromophenylsulphonyl chloride (1.02 g) was added to a mixture of 1-[1-(3-fluoro-4-pyridyl)-piperidin-4-ylcarbonyl]piperazine hydrochloride (1.22 g) and triethylamine (3.70 ml) in dichloromethane (45 ml) at 0° C. The solution was stirred at ambient temperature for 18 hours. The solution was diluted with dichloromethane and washed with water, dried (Na2SO4) and evaporated. The residue was purified by chromatography eluting with 2% methanol in dichloromethane. Recrystallisation from ethyl acetate/hexane gave 1-(4-bromophenylsulphonyl)-4-[1-(3-fluoro-4-pyridyl)piperidin-4-ylcarbonyl]piperazine (1.24 g) as a solid.
WORKUP
后处理
- washwashed with water
- dry with materialdried (Na2SO4)
- customevaporated
- customThe residue was purified by chromatography
- washeluting with 2% methanol in dichloromethane
- customRecrystallisation from ethyl acetate/hexane