Abstract: A novel convenient method for the synthesis of ¹³C-methanol was described. ¹³C-methanol was prepared by means of catalytic hydrogenation, and then as synthesized methanol solution was further purified in a microscale high-efficient rectification column. The chemical purity of ¹³C-methanol was more than 99.5%. The synthetic route was featured by mild conditions and high yields of more than 90% based on isotopic substrate consumed. The product was characterized by GC-MS and ¹H NMR, and the ¹³C abundance of ¹³C-methanol was more than 97%. Compared with the raw materials, the reduction of relative isotopic abundance of product was less than 1%.