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Decomposition of acetone cyanohydrin is the first-step reaction for preparing (S)-α-cyano-3-phenoxybenzyl alcohol (CPBA) by the one-pot method in organic media. Considering the compatibility of bio-catalysts with chemical catalysts and the successive operation in the bioreactor, anion exchange resin (D301) wasused as catalyst for this reaction. External diffusion limitation was excluded by raising rotational speed to higherthan 190r@min-1 in both solvents. Internal diffusion limitation was verified to be insignificant in this reactionsystem. The effect of acetone cyanohydrin concentration on the reaction was also investigated. An intrinsic kineticmodel was proposed when the mass transfer limitation was excluded, and the average deviation of the model is10.5%.