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
2-Ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridine (0.85 g, 4.8 mmol) was dissolved in DMF (15 mL), and the solution was added with potassium tert-butoxide (0.60 g, 5.3 mmol) at 0° C. followed by stirring for 10 min. Thereto was added a solution of the residue obtained above in DMF (8 mL), and the mixture was stirred at room temperature for 2 hr. Ethyl acetate was added to the mixture, the organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=3/1-1/3) to give (E)-[2-(2-ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridin-3-yl)methyl-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene]acetonitrile (1.28 g, 63%).
WORKUP
后处理
- additionThereto was added a solution of the residue
- stirringthe mixture was stirred at room temperature for 2 hr
- washthe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=3/1-1/3)