反应详情

To a heterogeneous solution of 2-[3-methyl-4-(2,2,2-trifluoroethoxy)pyridin-2-yl-methanesulfinyl]-1H-benzimidazole (LANSOPRAZOLE, 800 mg, 2.17 mmol) and 3 mL of Et3N in 20 mL of CH2Cl2 was added the chlorosulfonyl ester (Intermediate 60, 1.2 g, 2.60 mmol, 1.2 eq). About 1 g of solid NaHCO3 was added after the chlorosulfonyl ester has dissolved completely in the reaction mixture. The mixture was stirred at room temperature 1 h. Thereafter the solvent was removed by evaporation and the residual oil was purified by column chromatography (silica gel, CH2Cl2 to 1% MeOH in CH2Cl2) to give Intermediate 63 (1.2 g, 70%) as an off-white foam.

1. dissolutionhas dissolved completely in the reaction mixture
2. customThereafter the solvent was removed by evaporation
3. customthe residual oil was purified by column chromatography (silica gel, CH2Cl2 to 1% MeOH in CH2Cl2)