反应详情

温度

70 °C

180 mg (0.743 mmol) of ethyl 4-[(pyridine-4-yl)amino]benzoate was dissolved in 5 ml of concentrated hydrochloric acid, and the solution was stirred at 70° C. for 15 hours. The solvent was evaporated, and the residue was dissolved in 5 ml of dichloromethane. 0.23 ml (1.64 mmol) of triethylamine, 156 mg (0.82 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, 208 mg (0.82 mmol) of 1-hydroxybenzotriazole and 199 mg (0.82 mmol) of 3-(2-aminoethoxy)benzonitrile hydrobromide were added to the solution, and they were stirred for 16 hours. The reaction liquid was diluted with water. After the extraction with ethyl acetate, the organic layer was successively washed with water, 1 N sodium hydroxide and saturated aqueous NaCl solution, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was purified by the silica gel column chromatography to obtain the title compound.

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in 5 ml of dichloromethane
3. stirringwere stirred for 16 hours
4. customThe reaction liquid
5. extractionAfter the extraction with ethyl acetate
6. washthe organic layer was successively washed with water, 1 N sodium hydroxide and saturated aqueous NaCl solution
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was evaporated
9. customthe residue was purified by the silica gel column chromatography