反应详情

To a solution of methyl 3-(chlorosulfonyl)-4-methoxybenzoate 40 (1.002 g, 3.8 mmol) in CH2Cl2 (20 mL) at 0° C. was added pyridine (0.46 mL, 6 mmol) and morpholine (0.395 mL, 5 mmol). The reaction mixture was warmed to room temperature, stirred for 30 min, and diluted with EtOAc. The organic phase was washed with NaHCO3 (1×), brine (1×), dried over MgSO4, filtered, and concentrated in vacuo. Purification by flash column chromatography on silica gel (eluted with 0% to 20% EtOAc in CH2Cl2) gave methyl 4-methoxy-3-(morpholinosulfonyl)benzoate 41 (0.970 g, 81% yield) as a white solid. Mass spectrum: calculated for C13H17NO6S 315.1. found 316.1 (M++1).

1. washThe organic phase was washed with NaHCO3 (1×), brine (1×)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customPurification by flash column chromatography on silica gel (eluted with 0% to 20% EtOAc in CH2Cl2)