Synthesis Technology of Methyl 4,4-Dinitrobutanoate

The methyl 4,4-dinitrobutanoate was obtained through Michael addition reaction using potassium salt of dinitromethane and methyl acrylate as reaction materials and tetrabutyl ammonium bromide as phase transfer catalyst.The structure of product was characterized by using1H-NMR,IR,UV-vis,mass spectrum,element analysis,and so on. The influence of reaction time,reaction temperature,catalyst amount and reactant ratio on yield of product was discussed through single factor method. The obtained optimal process conditions are as follows:using tetrabutyl ammonium bromide as phase transfer catalyst,reaction temperature is 35 ℃,n(methyl acrylate) : n(potassium salt of dinitromethane)=3 : 1,reaction time is 30 min,the mass of tetrabutyl ammonium bromide is 10% of potassium salt of dinitromethane mass. The yield of methyl gem-dinitrobutanoate product can reach 29% under the above optimal reaction conditions.