A cleaner process for preparation of alkylcarbonyloxyarylsulphonates,such as sodium 4-nonanoyloxybenzene sulfonate(NOBS),sodium 4-nonanoyloxynaphthalene-1-sulfonate,sodium 4-methacryloyloxybenzene sulfonate,sodium 4-methacryloyloxynaphthalene-1-sulfonate from acid anhydride and hydroxyarylsulphonate was reported,using sodium carbonate as an acid-captor and acetone as a solvent in a one-step process.The effects on the synthesis of NOBS were investigated.The results showed that yield of NOBS can reach 90.7% and its purity is 95.5%,respectively,under the optimal reaction conditions of,n(sodium 4-hydroxybenzenesulfonate)∶n(nonanoic anhydride)∶n(Na2CO3)=1∶1.3∶1.5,Me2CO as a solvent at 0 ℃~5 ℃ for 3 h.The structure of NOBS was characterized by IR and NMR.