Expansion of the tetrazine ring has first been found to occur when [1,2,4]triazolo[4,3‐b][1,2,4,5]tetrazines were allowed to react with CH‐active compounds in acetonitrile in the presence of triethylamine to give the unexpected series of 8,9‐dihydro‐7H‐[1,2,4]‐triazolo[4,3‐b][1,2,4,6]tetrazepine derivatives.
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