反应详情

To a solution of intermediate 3 (Example 5) (170 mg, 0.5 mmol) in anhydrous CH2Cl2 (8 mL), 2-chloro-4,6-dimethoxy-1,3,5-triazine (100 mg, 0.6 mmol) and 4-methylmorpholine (210 mg, 2 mmol) were added. After the reaction mixture was stirred at room temperature for 75 minutes, intermediate 2 (Example 3) (100 mg, 0.3 mmol) in anhydrous DMF (2.5 mL) was added into the solution. The solution was stirred under argon for overnight. The residue was dissolved in CH2Cl2 (20 mL) and washed with aqueous saturated NaHCO3 solution (20 mL). The aqueous layer was extracted with CH2Cl2 (50 mL). The combined organic phase was dried (Na2SO4) and the solvent was removed. The crude product was purified by silica gel column with CHCl3 to 10% CH3OH/CHCl3 as eluents to give the final product as a white solid (27 mg, 15%).

1. stirringThe solution was stirred under argon for overnight
2. washwashed with aqueous saturated NaHCO3 solution (20 mL)
3. extractionThe aqueous layer was extracted with CH2Cl2 (50 mL)
4. dry with materialThe combined organic phase was dried (Na2SO4)
5. customthe solvent was removed
6. customThe crude product was purified by silica gel column with CHCl3 to 10% CH3OH/CHCl3 as eluents