A novel one-step method for synthesis of paeonol,which was prepared from m-methoxyl phenol and acetic acid under catalyst of ZnCl2,with yield 68% was reported in this article.In addition,in order to improve water-solubility of paeonol,the glycosylation reactions of paeonol and 2,4-dihydroxyphenyl ethanone,which was metabolized intermediate of paeonol in organism,were carried out to modify their structures.Four glycosylation derivatives of paeonol and 2,4-dihydroxyphenyl ethanone reacted with α-bromide tetra-O-acetly-glucopyranose and α-bromide tetra-O-acetly-galactopyranose were synthesized,with yield 30-73%.Paeonol and its glycosylation derivatives were characterized by1HNMR.