ABSTRACT A convenient and efficient sp-sp carbon heterocoupling protocol based on the Negishi reaction was developed, in which the required zinc diacetylide was generated from 1, 4-bis (trimethylsilyl) butadiyne in situ and reacted with a bromoacetylene in apolar solvent mixtures. The method has been applied to the synthesis of unsymmetric glycosylated and symmetric diglycosylated oligo (ethynylene) s up to the octa (ethynylene).
