The effects of experimental conditions and acid catalysts on the removal of the trityl group of 1-alkyl-2-acyl-3-trityl-sn-glycerols to yield 1-alkyl-2-acyl-sn-glycerols have been investigated. Removal of the trityl protecting group was complicated by the concomitant migration of the 2-acyl moiety to yield the 1-alkyl-3-acyl-sn-glycerol isomer. The course of detritylation as well as the extent of the 2-acyl to 3-acyl migration under the various conditions used were followed by high performance liquid chromatography (HPLC). Optimum yields of the desired 1-alkyl-2-acyl-sn-glycerol (}90%) were obtained with a molar equivalent of boron trifluoride-methanol in methylene chloride at 22 C for five min.