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A process for the preparation of thiocyanato-bearing organoalkoxysilanes (D) represented by the general formula (3): NCS-R1-Si(OR2)nR33-n (wherein R1 is a divalent hydrocarbon group having 1 to 6 carbon atoms; R2 and R3 are each a monovalent hydrocarbon group; and n is 0 to 3), characterized by reacting a thiocyanate (A) represented by the general formula (1): MSCN (wherein M is alkali metal) with a haloalkylalkoxysilane (B) represented by the general formula (2): XR1Si(OR2)nR33-n (wherein X is halogeno; and R1, R2, R3, and n are each as defined above) in the presence of a phase transfer catalyst (C). (FIG.NIL).