We demonstrate how FlowNMR spectroscopy can readily be applied to investigate photochemical reactions that require sustained input of light and air to yield mechanistic insight under realistic conditions. The Eosin Y mediated photo-oxidation of N-allylbenzylamine is shown to produce imines as primary reaction products from which undesired aldehydes form after longer reaction times. Facile variation of reaction conditions during the reaction in flow allows for probe experiments that give information about the mode of action of the photocatalyst.

Covalently linked multiple calixarenes are valued in supramolecular chemistry. This work reports an easy and versatile synthetic route to covalently linked double and triple calix[4]arene and calix[6]arenes by a novel DMF‐controlled selective alkylation of a convenient and readily available upper‐rim dimethylaminomethyl‐substituted tetrahydroxy and hexahydroxy calix[4]arene and ‐[6]arenes. Synthetic routes to upper‐rim functionalised redox active disulfide‐linked double‐, tetra‐ and peptidohybrid‐calixarenes employing either redox chemistry (CH2SH) or thiolates (CH2S−) are also opened up from the same key starting material.

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