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Initial formation of thiocyanogen [(SCN)2] by controlled potential anodic oxidation of NH4SCN in formic acid‐LiClO4 followed by addition of alkene as a second step, has been investigated for eight alkene derivatives. The results indicate that major products from most of the alkenes studied are addition products involving thiocyanate and formate groups. Also minor products of addition of isothiocyanate and thiocyanate groups, and allylic thiocyanates as substitution derivatives, were formed.