m-Chlorosulfonylbenzoyl chloride were prepared by the reaction of benzotrichloride with chlorosulfonic acid.The optimum reaction conditions at 120 ℃ for 2 h were as follows: benzotrichloride was 10 mL(70 mmol);n(benzotrichloride) ∶n(chlorosulfonic acid)=1 ∶2.The yield was 81% under the optimum reaction conditions.