A novel and efficient method for preparation of methylthio arylbutadiynes (Ar-C≡CC≡C-SCH 3 ) was described, and a series of compounds have been expediently obtained by the one-pot protocol starting from methylthiomethyl phenyl sulfone (MP-S) and arylpropargyl aldehydes. The mechanism was discussed on the basis of trapping and characterization of key intermediates. The results from experiments indicated that the reaction involved the initial ...