Amorphous (noncrystalline) cellulose was prepared by dissolving cotton hydrocellulose in the dimethylsulfoxlde-paraformalde-hyde solvent system and regenerating the cellulose by slow addition of the resultant raethylol cellulose solution to stirred 0.2M sodium alkoxide in methanol :2-propanol (1:1 vol.). The regenerated celluloses, essentially devoid of residual methylol substic-uents (ca. 0.002 ra.s.), had x-ray diffractograras, Raman spectra, and solid-state13C-n.m.r. spectra characteristic of amorphous cellulose. In addition, 98–100% of the cellulose hydroxyl groups were accessible to proton exchange with deuterium oxide. For small scale (< 2 g) preparations, the d.p. and end group composition of the cellulose were essentially unaltered by the regeneration process.