Although the literature has shown that linear amyloses can be synthesized using enzymic techniques, the yields are only in the milligram range and the DPs in the hundreds. Using commercially available reagents, this study has developed a means of synthesizing amyloses with DPs up to 6100 in quantities approaching one gram. The synthesized amyloses are free of α-1.6 branches and have comparatively narrow molecular weight distributions. Additionally, this study demonstrates that DMSO is applicable for derivatizing amyloses to their carbanilates before gel permeation chromatographic analysis. The procedure developed is useful for derivatizing retrograded amyloses having limited solubility in pyridine. Furthermore, when DMSO is used, low temperature (-15℃) must be maintained to prevent amyloses from depolymerization.