The invention of a method for the synthesis of 1, 3-diols from the corresponding alcohols is described, via controlled, radical-mediated C− H functionalization. The sequence described herein entails near quantitative conversion to the corresponding trifluoroethyl carbamate, followed by a variant of the Hofmann− Löffler− Freytag reaction, cyclization, and hydrolysis to provide the 1, 3-diols. In addition to the 10 examples presented herein, the syntheses of ...