10 kg-grade production method of 2,6-diamino-1-oxopyrazine

Abstract

The invention discloses a 10 kg-grade production method of 2,6-diamino-1-oxapyrazine. The raw materials of the production method comprise the following components in parts by weight: main materials: 10-15 parts of iminodiacetonitrile, 10-15 parts of sodium nitrite, 10-15 parts of concentrated sulfuric acid, 50-80 parts of anhydrous methanol, 30-50 parts of triethylamine, and 10-15 parts of hydroxylamine hydrochloride; and auxiliary materials: 5-10 parts of potassium carbonate, 5-10 parts of anhydrous sodium sulfate, 5-10 parts of potassium bicarbonate, 80-100 parts of ethyl acetate, and 10-15parts of 70-80% ethanol. The purity of the DAPO prepared by the production method can reach to be 99% or more, and the melting point of the prepared DAPO is 270 DEG C or more, so that the final product LLM-105 prepared by the DAPO has excellent properties.

Description

Technical field [0001] The invention relates to the technical field of a method for synthesizing pyrazine compounds, and in particular to a method for producing 2,6-diamino-1-oxopyrazine in a 10-kilogram scale. Background technique [0002] LLM-105 is the world's leading third-generation safety explosive with excellent application prospects. The process route used in the prior art to synthesize LLM-105 includes: 1. Oxidizing 2,6-diamino-3,5-dinitrooxypyrazine (ANPZ) with trifluoroacetic acid to synthesize LLM-105, but this process The intermediate ANPZ in the route is very difficult to synthesize, and the price of trifluoroacetic acid is relatively high. In addition, the synthetic product of this process route is polluted and difficult to handle, the reaction temperature is also high, and the process is highly dangerous. 2. Using 2,6 dichloropyrazine to synthesize LLM-105 through four steps of substitution, nitration, ammoniation and oxidation. This process route consumes a larg...

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Problems solved by technology

The prior art process route for synthesizing LLM-105 includes: 1. Oxidation of 2,6-diamino-3,5-dinitrooxypyrazine (ANPZ) with trifluoroacetic acid to synthesize LLM-105, but the process The synthesis of the intermediate ANPZ in the route is very difficult, and the price of trifluoroacetic acid is relatively high, and the synthetic product of this process route is relatively polluted and difficult to handle, the reaction temperature is also high, and the process is highly dangerous

2. Using 2,6-dichloropyrazine to synthesize LLM-105 through four steps of substitution, nitration, ammoniation and oxidation. This process route consumes a lot of trifluoroacetic acid, the reaction temperature is high, the synthesis process conditions are complicated, and the nitration After the step is advanced, the subsequent steps are dangerous

3. Oxidation of ANPZ with hydrogen peroxide to synthesize LLM-105, its disadvantages are similar to the first method

However, in the prior art, the synthesis process for producing 2,6-diamino-1-oxopyrazine at the level of 100 grams is relatively mature, but the applicant found that if the 2,6-diaminopyrazine at the level of 100 grams is used When the synthesis process of amino-1-oxopyrazine is enlarged to produce kilogram-level 2,6-diamino-1-oxopyrazine, the amplification effect is more obvious. Although the yield of the product will be greatly improved, the melting point of the product Below 200°C, thin-layer chromatography shows that there are more impurities, resulting in lower purity of the obtained product, so that the 2,6-diamino-1-oxopyrazine product produced by the existing 100-gram-level synthesis process Unable to meet follow-up response requirements

In addition, it is easy to produce double-addition by-products in subsequent reactions

Therefore, the synthesis process of 2,6-diamino-1-oxopyrazine in the prior art has been unable to realize the stable synthesis of kilogram-level DAPO, which greatly hinders the large-scale popularization and application of the follow-up product LLM-105

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