反应详情

Compound 14 (0.250 g, 0.625 mmol) was dissolved in dichloromethane (5 mL), and triethylamine (0.131 mL, 0.939 mmol) and methanesulfonyl chloride (0.730 mL, 0.943 mmol) was added to the solution at 0° C., followed by stirring for 1 hour. The reaction mixture was added with a saturated aqueous sodium hydrogen carbonate solution, and diluted with chloroform, then washed with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was dissolved in dichloromethane (5 mL), and 1-methylpiperazine (0.208 mL, 1.87 mmol) and triethylamine (0.870 mL, 0.623 mmol) was added to the solution, followed by stirring at room temperature overnight. The reaction mixture was diluted with chloroform, and washed with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain Compound 15 (0.0900 g, yield 30%).

1. washwashed with water and saturated brine
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. dissolutionThe residue was dissolved in dichloromethane (5 mL)
5. stirringby stirring at room temperature overnight
6. washwashed with water and saturated brine
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)