反应详情

温度

0 °C

4-(((1-(tert-Butoxycarbonyl)piperidin-4-yl)(4-chlorophenethyl)amino)methyl)benzoic acid synthesized in Step 2 was dissolved in DCM (5 mL/mmol) and DIPEA (3 equiv) and methanesulfonamide (2 eqs) were added. The reaction mixture was cooled to 0° C. and TFFH (1.2 eq) was added in one portion. The reaction mixture was stirred at 0° C. for 6 hours and then for 15 hours at room temperature. Ethyl acetate (15 mL/mmol) was added and the solution was washed sequentially with 5% citric acid (2×), 5% NaHCO3 (2×) and brine (2×) and was dried over MgSO4. The drying agent was filtered off and the solvents were evaporated in vacuo. The crude product was purified by silica gel chromatography.

1. waitfor 15 hours at room temperature
2. washthe solution was washed sequentially with 5% citric acid (2×), 5% NaHCO3 (2×) and brine (2×)
3. dry with materialwas dried over MgSO4
4. filtrationThe drying agent was filtered off
5. customthe solvents were evaporated in vacuo
6. customThe crude product was purified by silica gel chromatography