Preparation method of aminoation reagent 2,4,6-trimethyl-benzenesulfonamide and benzenesulfonamide derivatives

Abstract

The invention discloses a preparation method of an aminoation reagent 2,4,6-trimethyl-benzenesulfonamide and benzenesulfonamide derivatives. The preparation method comprises the following specific steps: taking ethyl acetate, hydroxylamine hydrochloride and potassium carbonate at a molar ratio of 2:(3-5):(6-7), firstly mixing ethyl acetate and hydroxylamine hydrochloride in an organic solvent to have a reaction; then, adding potassium carbonate into the above solution and further stirring to have the reaction; filtering, extracting, drying and removing the solvent to obtain white solids; reacting the white solids with a sulfonyl chloride derivative and triethylamine and then pouring the reaction liquid into an ice-water mixture to separate out white precipitate; reacting the white precipitate with 70% perchloric acid in an organic solvent and then pouring into ice water to separate out solids; and dissolving the solids, drying and removing the solvent to obtain a needle-like benzenesulfonamide derivative. The preparation method disclosed by the invention is simple; the prepared aminoation reagent can be applied to the field of energy-containing materials.

Description

technical field [0001] Embodiments of the present invention relate to the preparation of energetic materials, which belong to the field of organic synthesis. More specifically, embodiments of the present invention relate to an ammoniating reagent 2,4,6-trimethylbenzenesulfonamide and benzenesulfonamide derivatives Preparation. Background technique [0002] Energetic compounds are widely used in explosives, pyrotechnics, and propellants. At present, nitro groups and N-O bonds are often introduced into energetic compounds to increase energy, but with the increase in energy, the sensitivity also increases. Therefore, introducing an amino group into the molecular structure and forming a hydrogen bond with the nitro group or oxygen atom in the molecule can effectively reduce the sensitivity of the energetic compound and increase the stability of the molecule, forming a compound that can interact with 1,3,5-triamino -2,4,6-trinitrobenzene (TATB) comparable insensitive explosives...

AI Technical Summary

Problems solved by technology

But the synthetic method report of amination reagent is seldom (J.Houben and E.Schmidt, Chem.Ber.,46,3616(1913); J.Org.Chem.,38,1239-1241,1973), aftertreatment The method of vacuum distillation is used for purification at 60°C / 14Torr., and the ammoniation reagent is divided into three steps, and each step needs to be recrystallized for purification. The whole process is cumbersome and requires high reaction conditions. The price is high, resulting in a high cost of raw materials for the preparation of ammoniation reagents, about 8,000 yuan / kg-10,000 yuan / kg

At present, there are few reports on the preparation method of low-cost, one-step synthesis of ammoniating reagents, and the use of aminating reagents to introduce amino groups into energetic molecules to reduce explosive sensitivity, increase molecular density, and improve molecular stability.

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