A practical and eco-friendly method for the clean preparation of a variety of Z-β-thiocyanate alkenyl esters via lactic acid-catalyzed multicomponent hydrothiocyanation reaction was established. In the subgram-scale synthesis, Z-β-thiocyanate alkenyl esters were exclusively generated, and the product could be easily isolated in high purity via extraction. In the large-scale synthesis, the pure products could be simply collected through liquid–liquid separation. The eco-friendly lactic acid played a dual function in the transformation, serving as recyclable biomass catalyst and recyclable reaction medium.

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