Under nitrogen protection, 2-methyl-1-propanethiol (200 mg, 2.22 mmol) was dissolved in acetonitrile and cooled to 0 °C. N-chlorosuccinimide (561 mg, 5.5 mmol) and sulfonyl chloride (0.45 ml, 5.5 mmol) were added sequentially. The reaction mixture was kept stirred at 0 °C for 3 hours. After completion of the reaction, it was diluted with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layers were combined, washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure to give 2-methylpropanesulfonyl chloride (293 mg, 95% yield).