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
Potassium carbonate (26.5 mmol) and N-methylpiperazine (6.36 mmol) was added to a solution of tert-butyl 2-((methylsulfonyloxy)methyl)-6,7-dihydrothieno-[3,2-c]pyridine-5(4H)-carboxylate (5.3 mmol) in toluene (30 ml). The reaction mixture obtained was heated under reflux for 16 hours. The reaction temperature was then reduced to 25° C. and the reaction mixture was diluted with ethyl acetate. The reaction mixture was washed with water and saturated sodium chloride solution and dried over sodium sulfate. After the solvent had been removed under reduced pressure, the crude product obtained was purified by column chromatography (5% methanol in methylene chloride). The desired product was obtained in a yield of 50%.
WORKUP
后处理
- customThe reaction mixture obtained
- temperaturewas heated
- temperatureunder reflux for 16 hours
- customwas then reduced to 25° C.
- washThe reaction mixture was washed with water and saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- customAfter the solvent had been removed under reduced pressure
- customthe crude product obtained
- customwas purified by column chromatography (5% methanol in methylene chloride)