A new type of lambda6-sulfanenitrile with an SN triple bond at both ends, Ph2S(=N-(Ph2)S[triple bond]N)2 (5), was prepared in excellent yield from the one-pot synthesis of diphenylsulfimide (Ph2SNH) with fluoro(diphenyl)-lambda6-sulfanenitrile (Ph2FSN) in the presence of 1,8-diazabicyclo[5.4.0]undec-7-ene. Its molecular structure was determined by X-ray crystallographic analysis. Compound 5 reacted further with methyl triflate and trifluoromethanesulfonic anhydride to afford the corresponding bis-N-methylated and -N-sulfonated compounds.

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