The nucleophilic addition reaction was happened between 2-pyrrolidone and acrylonitrile in the toluene solvent using the PTC and sodium hydroxide respectively as phase transfer agent and catalyst. The nitrile fraction which seemed as pale yellow liquid was obtained by rectification. The effect of types and amount of PTC on gas chromatographic purity and yield of product were studied. The results showed that a better product could be obtained by using BTEAC as the catalyst compared to the CTAB and TBA. The optimum experimental condition was determined by the orthogonal experimental method. The yield was as high up to 94.2% when the quality score of BTEAC accounted for 0.5% of the total feeding mass, the concentration of aqueous solution of sodium hydroxide was 10%, acrylonitrile excessed 5%, gas chromatographic purity of the product was 98.5%.