The synthetic method of 2,3-dimethyl-2,3 dinitrobutane

Abstract

The invention discloses a synthetic method of 2,3-dimethyl-2,3-dinitrobutane. The synthetic method comprises the following steps that 1, acetoxime, water, and catalyst modified titanium silicalite (TS)-1 are added into a reaction container at room temperature; 2, aqueous alkali and hydrogen peroxide are added dropwisely into the reaction system obtained by the previous step at a temperature of 60to 90 DEG C with stirring; the pH of the reaction system is kept in a range of 8 to 10; and a mol ratio of hydrogen peroxide and acetoxime is in a range of 1 to (3: 1); 3, after dropwiseaddition, themixture obtained from the step 2 undergoes a reaction at a temperature of 60 to 90 DEG C for 0 to 2 hours; 4, reaction products obtained from the step 3 is cooled to room temperature and then is subjected to a filtration or a centrifugation process thus modified TS-1 is separated from the cooled reaction product and mother liquor is obtained; the modified TS-1 is washed by acetone; washing liquidis collected; and the collected washing liquid is added into the mother liquor; and 5, the mother liquor containing the collected washing liquid is subjected to a distillation process at a temperature less than or equal to 80 DEG C so that acetone in the reaction system is removed; the mother liquor treated by the distillation process is cooled and filtrated; and filter residues are washed by water to form 2,3-dimethyl-2,3-dinitrobutane products. Raw materials adopted by the synthetic method have the advantages of good safety and low cost. 2,3-dimethyl-2,3-dinitrobutane synthesized by the synthetic method has the advantages of less impurities and high product quality.

Description

technical field [0001] The invention relates to the technical field of compound synthesis methods, in particular to a synthesis method of 2,3-dimethyl-2,3-dinitrobutane. Background technique [0002] 2,3-Dimethyl-2,3-dinitrobutane (DMNB) is an important organic intermediate with a wide range of uses. For example, it has special functions and uses as a tracer for explosives. The International Civil Aviation Organization (ICAO) issued a document in 1991, which mandated that tracers be added to plastic explosives to facilitate the detection of explosives at airports. 2,3-II Methyl-2,3-dinitrobutane can replace nitrotoluene as a tracer. 2,3-Dimethyl-2,3-dinitrobutane is also one of the key raw materials for the synthesis of 2-substituted-1,3-dioxo-4,4,5,5-tetramethylimidazolines , this kind of substance has specific capture performance for NO, and has important application in medicine. In addition, 2,3-dimethyl-2,3-dinitrobutane is also one of the important raw materials for ...

AI Technical Summary

Problems solved by technology

However, this method also uses raw materials such as dangerous chemicals 2-nitropropane and NaH, and also uses expensive ammonium cerium nitrate, resulting in increased synthesis costs.

[0009] In summary, the synthetic method of 2,3-dimethyl-2,3-dinitrobutane of the prior art all takes 2-nitropropane as raw material, and uses more dangerous chemicals, to Safe production has great hazards, and contains many impurities and poor product quality

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