1039020-81-9

53531-45-6

1039020-81-9

The general procedure for the synthesis of methyl 2-(chlorosulfonyl)-5-nitrobenzoate from the compound (CAS:53531-45-6) was as follows: first, 5.1 g (12 mmol) of 2,2'-thio-bis(4-nitrobenzoate) obtained by extraction in step (2) was dissolved in a reaction solution containing 5.04 g (60 mmol) of 95% ammonium nitrate and 42.3 mL of TMSCl (96 mmol) in 60 mL of dichloromethane to prepare the reaction solution. The reaction solution was transferred to a closed glass tube and the reaction was stirred at 50 °C for 15 to 24 h, during which the reaction progress was monitored by TLC. After completion of the reaction, the reaction solution was cooled to room temperature and filtered. Subsequently, the filtrate was washed sequentially with 200 mL of water and 100 mL of saturated brine. The filtrate was collected, dried with anhydrous Na2SO4, concentrated overnight under reduced pressure, and distilled to remove the solvent, resulting in 2.754 g of solid product, 2-methoxycarbonyl-4-nitrobenzenesulfonyl chloride, from the filtrate.