The catalytic behavior of concentrated heteropolyacid solution in acylation of anisole with acetic anhydride has been investigated under the reaction conditions such as molar ratio of anisole to acetic anhydride, reaction temperature and mass ratio of reactant to catalyst. When the molar ratio of anisole to acetic anhydride is changed from 2∶1 to 1∶1, the yield of methoxyacetophenone (MOAP) increases a little, but when it is changed from 1∶1 to 1∶2, the yield has a greater increase from 15% to 30%. The yield of MOAP at the reaction temperature of 363 K doubles that at 333 K. The highest yield is obtained when the mass ratio of reactant to catalyst is 12 8. The conclusion is therefore that the heteropolyacid in acetic acid can effectively catalyze the acylation of anisole with acetic anhydride, and its activity and selectivity are comparable to those of acid clay and molecular sieve.