反应详情

温度

25 °C

The oily residue of the compound of Example 9 was dissolved in 5 mL of DMF, cooled to 0° C. and neutralized with 1 mL of TEA. To the solution was added BnSO2Cl (397 mg, 2.0 mmol) and the solution was stirred at 0° C. for 3 h and 25° C. for 3 h. DMF was removed and residue was dissolved in 100 mL of EtOAc and 20 mL of water. The organic layer was separated, washed with sat. NaHCO3 (10 mL), water (10 mL), 1 N HCl (10 mL) and sat. NaCl (3×10 mL), dried with MgSO4, filtered and evaporated. The solid residue was purified by column chromatography on silica gel (EtOAc) to give the title compound (328 mg, 30% yield) as a powder. ES—MS (M+H)+630.5

1. customDMF was removed
2. dissolutionresidue was dissolved in 100 mL of EtOAc
3. customThe organic layer was separated
4. washwashed with sat. NaHCO3 (10 mL), water (10 mL), 1 N HCl (10 mL) and sat. NaCl (3×10 mL)
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. customevaporated
8. customThe solid residue was purified by column chromatography on silica gel (EtOAc)