The Synthesis of 2-Oxo-1-Pyrrole Alkyl Propionitrile

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%.

Process Research of 1-(3,4-Dichloropheny)-3-Methyl-Pyrazolone-5-one Synthesis

The new process of 1-(3,4-dichloropheny)-3-methyl-pyrazolone-5-one (34DCPMP) synthesis had been discovered, which using 3,4-dichloro phenylhydrazine hydrochloride(DCPH) and ethyl acetoacetate as the raw material , The product was obtained by the route during cyclization in aqueous medium. The structure of products was confirmed by 1HNMR, 13CNMR and IR. The effects of factors on the yield of products were investigated. It was found that the yield of 34DCPMP can reach 98.7% under the optimal reaction condition of n(34DCPH):n(ethyl acetoacetate) with 1:1.1, n(34DCPH):n(Na2SO3) with 1.3:1 at 80°C, and pH 7.5 for 3h. The chromatographic purity can be higher than 98.2%.