27277-00-5Relevant articles and documents
Technology for three-innovation synthesis of 2-amino-5-methyl-4-oxo-3-n-propyltriazolopyrimidine
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Paragraph 0015; 0029-0040, (2019/11/29)
The invention discloses a technology for synthesizing 2-amino-5-methyl-4-oxo-3-n-propyl-6H-triazolo-[1,5-a]pyrimidine. Methyl methacrylate and bromine are firstly subjected to an addition reaction toprepare methyl 2,3-dibromo-2-methylpropanoate, and then the methyl 2,3-dibromo-2-methylpropanoate and sodium methylate are etherified in a new suitable solvent to prepare methyl 3,3-dimethoxy-2-methylpropionate etherate; the etherate and 3,5-diamino-1,2,4-triazole, prepared from hydrazine hydrate and dicyandiamide under the catalysis of an acid, are condensed at an intermediate temperature of about 115 DEG C under the catalysis of an organic base to obtain a pyrimidotriazole compound; and the pyrimidotriazole material liquid and 1-chloropropane undergo a direct alkylation reaction in an inorganic or organic bas and a new solvent to obtain the 2-amino-5-methyl-4-oxo-3-n-propyl-6H-triazolo-[1,5-a]pyrimidine. The technology is improved by the three major innovations of improving the catalyticsynthesis conditions of the condensation ring closure of the pyrimidotriazole, optimizing the alkylation substitution reaction and the process technology of the pyrimidinetriazole and innovating theraw material of an alkylation reagent, so the technology has the advantages of great improvement of the yield, simplicity in operation, mild reaction conditions, and safety to devices and human bodies, the total yield of methyl methacrylate can reach 46.5% or above, and the obtained product has a white color and a good crystalline state, and has a content of 99% or more.
A triazole pyrimidone preparation method
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Paragraph 0014; 0024-0047, (2019/04/04)
The invention belongs to the technical field of organic synthesis, particularly discloses a triazole pyrimidone preparation method, comprises the following steps, in under the action of the phase transfer catalyst, pyrimidine triazole, bearing-displacement, inorganic base in an organic solvent in the reaction, the reaction temperature is 20 - 170 °C, the reaction time is 4 - 8 h, adding water and ethyl acetate is dissolved solid, liquid after the ethyl acetate extraction, the combined extract to dryness, after ethanol heating dissolved solids, cooling crystallization, filtering, washing, and the filtrate is concentrated, the cooling crystallization, filtered washing, the combined product, the product is obtained. The discharge can be obtained by direct crystallization product quality is good, the content is high, can be up to 99.5%, high yield, can be up to 83.5% - 86.5%, the reaction conditions are more stable, mild, the operation is simplified.
Preparation method of paraquat vomitive, namely triazole pyrimidone
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Paragraph 0028; 0029; 0030; 0031; 0032; 0033; 0034-0044, (2018/03/28)
The invention discloses a preparation method of a paraquat vomitive, namely triazole pyrimidone (namely 2-amion-6-methyl-4-n-propyl-[1,2,4]-triazol[1,5-a] pyrimidine-5-ketone). The preparation methodcomprises the following steps: taking 2-amion-6-methyl-[1,2,4]-triazol[1,5-a] pyrimidine-5-ketone and n-propyl bromide as the raw materials, taking an organic alkali as an acid binding agent, reactingin an organic solvent I, obtaining a solution containing the 2-amion-6-methyl-4-n-propyl-[1,2,4]-triazol[1,5-a] pyrimidine-5-ketone, wherein the reaction temperature is 60-80 DEG C, and the reactiontime is 5-8 hours; and distilling the solution to recycle the organic solvent I, adding water and an organic solvent II into an obtained residue to extract, separate and recrystallize, and obtaining 2-amion-6-methyl-4-n-propyl-[1,2,4]-triazol[1,5-a] pyrimidine-5-ketone.