The 1,2,3,5-tetra-O-benzoyl-2-C-methyl-βD-ribonfuranose was synthesized from D-fructose by four steps, which were lactonization, acylation, reduction, and acylation, the overall yield was 10.6%. The characterization methods of 1HNMR、13C-NMR and MS were applied to confirm the structures of intermediates and product. Combining with the reduction condition, the best raw material for synthesizing 2-C-Methyl-D-ribonic-γ-lactone were D-fructose and CaO. The conclusion that the best reductant for 2,3,5-Tri-O-benzoyl-2-C-methyl-βD-ribofuranose is Red-Al was obtained by comparing using three different reductant as LiAlH4, NaBH4 and Red-Al and the yield can up to 96.20%.Through single factor experiments determented that triethylamine was the best acid binding agent for acylation reaction and the yield can up to 75.84%.