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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 200 mg 4-{6-[3-(4-fluorophenyl)-1-trityl-1H-4-pyrazolyl]imidazo[1,2-a]pyridin-3-yl}phenol (compound in Example 14), 232 mg ethyl 7-bromoheptanoate, 6 mg sodium iodate, 68 mg potassium carbonate, and 15 mL N,N-dimethylformamide was stirred overnight at 80° C. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated, then washed with water, an aqueous saturated sodium thiosulfate, an aqueous solution of sodium chloride (×2) and brine, and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was evaporated. The resulting residue was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 157 mg of the title compound as a pale brown amorphous.
WORKUP
后处理
- customthe organic layer was separated
- washwashed with water
- dry with materialan aqueous saturated sodium thiosulfate, an aqueous solution of sodium chloride (×2) and brine, and dried over anhydrous sodium sulfate
- filtrationThe drying agent was filtered off
- customthe filtrate was evaporated
- customThe resulting residue was purified by NH silica gel column chromatography (ethyl acetate/hexane)