反应详情

3.0 mg of 4-benzylamino-6-[4-methoxybenzyl-(6-morpholinopyridin-3-yl)amino]pyridine-3-carboxyamide was dissolved in 0.5 mL of methylene chloride, to which 0.5 mg of trifluoroacetic acid was added, stirred at room temperature for 4 hours, and further heated at reflux at 70° C. for 8 hours. After cooling, the solvent was evaporated, saturated sodium bicarbonate in water was added to the residue, extracted with chloroform, the extract was washed with saturated saline, and dried on anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by silica gel thin layer chromatography (chloroform:methanol=10:1) and silica gel thin layer chromatography (chloroform:ammonium-saturated methanol=10:1) to obtain 1.2 mg (4 steps, yield 3%) of the title compound as a light brown solid.

1. additionwas added
2. temperaturefurther heated
3. temperatureat reflux at 70° C. for 8 hours
4. temperatureAfter cooling
5. customthe solvent was evaporated
6. additionsaturated sodium bicarbonate in water was added to the residue
7. extractionextracted with chloroform
8. washthe extract was washed with saturated saline
9. dry with materialdried on anhydrous sodium sulfate
10. customThe solvent was evaporated
11. customthe residue was purified by silica gel thin layer chromatography (chloroform:methanol=10:1) and silica gel thin layer chromatography (chloroform:ammonium-saturated methanol=10:1)