AbstractAn improved method has been used to synthesize perfluoroazo‐2‐propane. Pyrolysis over the temperature range 450–514 K in a static system has been shown to be a homogeneous, first‐order process. No pressure dependence was observed in the presence of excess inert gas (SF6). The only products were nitrogen and perfluoro‐2,3‐dimethylbutane. The rate constant (k) for the decomposition process is given by:\documentclass{article}\pagestyle{empty}\begin{document}$$ \log \left({{k \mathord{\left/{\vphantom {k s}} \right. \kern-\nulldelimiterspace} s}^{- 1}} \right) = 16.7 \pm 0.2 - {{\left({9856 \pm 109} \right)} \mathord{\left/{\vphantom {{\left({9856 \pm 109} \right)} T}} \right. \kern-\nulldelimiterspace} T} $$\end{document}These results lead to a straightforward mechanism for the decomposition processThe results are compared with those for other azo compounds. © 1994 John Wil