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Photolabile linkers are regarded as chemically stable and are able to be cleaved under mild conditions without inducing destructive reactions on target molecules. o-Nitrobenzyl-based linkers have been widely employed in solid-phase synthesis. Recently, several o-nitrobenzylic-based photolabile resins retaining various modifications at the reducing end of glycans after photocleavage were developed by our group. In this work, the synthesis of three distinct o-nitrobenzylic derivatives is described, and the immobilization of the linkers onto commercial Merrifield resin is carried out. Subsequently, detailed procedures for loading determination and photocleavage are provided.