Due to the previous unsuccessful attempt with Py•SO3, DMF•SO3 complex was used for the sulfation of xylobios. The sulfation of xylobios with DMF•SO3 complex was carried out between -15 to 0 °C for two hours affording xylobiose hexasulfate and xylobiose pentasulfate, a reduced sugar, which was formed via hydrolysis of hexasulfate substrate (Scheme 14). Scheme 14. The sulfation reaction of xylobios using DMF•SO3 complex affording xylobiose hexasulfate and pentasulfate.