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The mad cow disease, bovine spongiform encephalopathy, is a deadly, neurodegenerative disease in cattle, which causes spongy in the brain and spinal cord. Many scientists think the disease as transmittable to human beings by taking the brain and spinal cord of infected cattle. In an effort to study important biological functions of the mad cow disease and to develop the chemotherapy agents, it is essential to synthesize the glycosyl phosphatidyl inositol (GPI) anchor, which connects scrapie prion protein via their C-terminus to eukaryotic cell membranes. In the present work, the synthesis of {a-D-Manp-(1→2)-a-D-Manp-(1→2)-a-D-Manp-(1→6)-[b-D -GalNAcp-(1→4)]-a-D-Manp}, a suitably protected form of pentasaccharide unit of GPI anchor of scrapie prion protein was achieved by assembling of five monosaccharide building blocks with careful stereo- and position-manipulations. The ready accessibility of all starting materials, the high yields obtained in all reaction steps, including the glycosylation reactions which were carried out with trichloroacetimidates, provide an excellent basis for further successful syntheses in this field.