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A convenient one-pot synthesis of stable phosphorus ylides by the condensation of triphenylphosphine with dialkyl acetylenedicarboxylate and CH acids, such as penta-2,4-dione or diethyl propane-1,3-dioate, in the presence of β-cyclodextrin as a catalyst (to increase the solubility of the reactants in water) without using toxic organic solvents was proposed. This methodology is of interest due to the use of water as a solvent, thus minimizing such factors as the cost, operational hazards, and environmental pollution.