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The preparation and acid catalysed hydrolysis of a number of isoxazolinyldioxepins is reported. Individual diastereoisomer pairs were isolated b y column chromatography and shown t o differ significantly in their hydrolytic stability at acidic pH. The crystal structures of one diastereoisomer pair reveal that conformational differences induce a selective stereoelectronic effect at the acetal centre of the more hydrolytically labile isomer, while the less labile isomer shows no such selectivity.In our search for biologically active molecules we came across a number of isoxazolinyldioxepin derivatives of general structure (A), which differed in the nature of the substituent 'X'. We were Table 1. Melting points and elemental analyses of the isoxazolinyldioxepin derivatives (1)glO).

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