Perdeuterated 2, 4-dinitroanisole and preparation method thereof

Abstract

The invention relates to perdeuterated 2, 4-dinitroanisole and a preparation method thereof, and belongs to the technical field of synthesis of deuterated energetic materials. Deuterated anisole is used as a raw material, and the raw material is relatively easy to obtain; the crude product only needs one purification step, the purity of the obtained product is high, and a standard solution for analysis can be directly prepared to serve as a deuterated internal standard substance for researching the metabolic process. Compared with common 2,4-dinitroanisole, the perdeuterated 2,4-dinitroanisoleprovided by the invention has the advantages that the crystal density is increased; meanwhile, the explosion heat is also increased. The perdeuterated 2,4-dinitroanisole can be used as an insensitivefusion casting carrier explosive, and the solubility of the sample to hexogen at 100 DEG C is increased to 17 g of hexogen dissolved in every 100 g of perdeuterated 2,4-dinitroanisole. The method isrelatively simple to operate, relatively short in reaction period and relatively high in product purity and yield, the preparation of the perdeuterated 2,4-dinitroanisole is realized, and a referenceis provided for industrial production of the perdeuterated 2,4-dinitroanisole.

Description

technical field [0001] The invention relates to a fully deuterated 2,4-dinitroanisole and a preparation method thereof, belonging to the technical field of synthesis of deuterated energetic materials. Background technique [0002] 2,4-Dinitroanisole is currently the most researched insensitive melt-cast carrier explosive, and it has received widespread attention since it came out in 1849. Compared with the common melting and casting explosive TNT, the shock wave sensitivity and thermal sensitivity of 2,4-dinitroanisole are relatively low. After melting and casting, the mechanical properties of the explosive are relatively ideal, the elasticity and toughness are good, the strength is high, and it is not easy to appear inside cracking etc. Moreover, 2,4-dinitroanisole is also an important chemical dye intermediate for the production of scarlet base RC (2-methoxy-5-nitroaniline hydrochloride). In addition, 2,4-dinitroanisole can also be used as an insecticide with excellent p...

AI Technical Summary

Problems solved by technology

In 2010, people such as Xia Xiaozhong used 2,4-dinitrobenzene as a raw material and synthesized 2,4-dinitroanisole with benzyltriethylammonium chloride as a phase transfer catalyst; although this method obtained 2, 4-Dinitroanisole, but the phase transfer catalyst is not easy to prepare, the cost is relatively high, and it is not suitable for large-scale use

In 2016, Liu Yan et al. used 1-chloro-2,4-dinitrobenzene (CDNB) as the raw material and KOH solution as the reaction medium to synthesize 2,4-dinitrobenzene in the next step without using a phase transfer catalyst. Anisole (Synthetic Chemistry, 2016,24(10):907-910); the optimal synthesis temperature range of this method is relatively narrow, and the product purity and yield decrease more when deviating from the optimal temperature, which is unfavorable for industrial operation

The method takes 2,4-dinitrochlorobenzene as a raw material, uses methanol as a solvent, and under mild conditions, reacts with sodium methylate to synthesize 2,4-dinitroanisole; the reaction cycle of the method is longer, no Conducive to industrial production

In addition, the products obtained by the above method are all non-deuterated 2,4-dinitroanisoles, and it is impossible to realize the preparation of all deuterated 2,4-dinitroanisoles by simply replacing the deuterated raw materials.

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