Abstract: The Haworth method was applied to the preparation of partially methylated glucose (glucoside)with Glc. MeGlc. and amylose as the starting materials. Products of various degree of methylation and at different positions were obtained under controlled reaction conditions. Further isolation and purification, were effected through RP-HPLC and the structure of each of the 19 derivatives was identified by GC, CI-MS as well as GC-M S. This method should be useful in preparing small amounts of partially methylated monosaccharides as standards for the structure study of carbohydrate chains in glycoconjugates.