A facile and efficient one‐pot strategy for the preparation of 1,2,3‐tri‐ and 1,1,2,3‐tetrasubstituted bis(guanidine)s by starting from from readily available bis(thiourea)s has been successfully developed. The reaction provides products that contain a range of terminal and bridging groups. After a simple workup procedure, the products were obtained in analytically pure and in good to excellent yields.
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