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
- 140 °C
PROCEDURE
实验过程
A mixture of 4-(2,3-dihydro-1H-imidazo[1,2-a]benzimidazol-1-yl)aniline (55 mg) and 2-chloro-3-nitropyridine (35 mg) in NMP (3 mL) was stirred at 140° C. overnight. After this time, the reaction mixture was cooled to ambient temperature, diluted with water (50 mL) and extracted with ethyl acetate (2×75 mL). The combined organic layers were washed with water (50 mL) then brine (50 mL), dried over sodium sulfate, and filtered and the filtrate was concentrated under reduced pressure. The residue obtained was purified by chromatography (silica, methylene chloride to 1:9 ethyl acetate/methylene chloride) to afford N-[4-(2,3-dihydro-1H-imidazo[1,2-a]benzimidazol-1-yl)phenyl]-3-nitropyridin-2-amine (34 mg) as a dark brown solid.
WORKUP
后处理
- temperatureAfter this time, the reaction mixture was cooled to ambient temperature
- extractionextracted with ethyl acetate (2×75 mL)
- washThe combined organic layers were washed with water (50 mL)
- dry with materialbrine (50 mL), dried over sodium sulfate
- filtrationfiltered
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue obtained
- customwas purified by chromatography (silica, methylene chloride to 1:9 ethyl acetate/methylene chloride)