Heat-induced solid-state decarboxylation of tetra(malonatemethylene) based cyclophane leads to its tetra(2-carboxyethyl) derivative in quantitative yield. This reaction provides more thermostable substance compared to the product of the same cyclophane decarboxylation in solution. The studied cyclophanes have been characterized by means of simultaneous thermal analysis involving thermogravimetry, differential scanning calorimetry, and mass spectrometry of evolved gases as well as fast scanning calorimetry, a method preferable to investigate the compounds with relatively low thermal stability.
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