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Selective benzoylation of HO-2 and HO-2′ of 4,6-O-benzylidene-α-D-glucopyranosyl 4,6-O-benzylidene-α-D-glucopyranoside with N-benzoylimidazole led to the exclusive formation of 2-O-benzoyl-4,6-O-benzylidene-α-D-glucopyranosyl 2-O-benzoyl-4,6-O-benzylidene-α-D-glucopyranoside. Oxidation of either the dibenzoate or the corresponding ditosylate with methyl sulphoxide-phosphorus pentaoxide gave the 3,3′-diulose, and subsequent reduction with borohydride gave the 3,3′diepimers having the allo-allo configuration. De-esterification and hydrolysis of the benzylidene substituents gave α-D-allopyranosyl α-D-allopyranoside. 相似文献