- Technology for three-innovation synthesis of 2-amino-5-methyl-4-oxo-3-n-propyltriazolopyrimidine
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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.
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Paragraph 0015; 0029-0040
(2019/11/29)
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- A preparation method of the emetic (by machine translation)
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The invention relates to the field of organic synthetic technology, in particular to a emetic preparation method, comprises the following steps: S1, 3 - methoxy methyl acrylic acid methyl ester preparation; S2, synthesis of [...]; S3, is the synthesis of third zuo; S4, and aldehyde; S5, closed-loop. This invention adopts the single melamine as the synthetic starting material, greatly reducing the cost, dicyandiamide as to effectively solve the problem of lack of raw material sources; solved in the prior art long reaction time, the reaction condition is sensitive, harsh, side reaction are numerous and complex, the use of expensive or difficult to prepare sodium of other reagents, reactions caused low overall yield, the product quality is poor, so that the synthesis process technology of the route is more stable, good reproducibility, high yield, the product quality is good, content can be up to 99.5%, the yield can reach 85.6%, has higher economic benefits. (by machine translation)
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Paragraph 0029; 0034; 0039; 0045; 0046; 0050; 0055; 0058
(2019/04/17)
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- A triazole pyrimidone preparation method
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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.
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Paragraph 0014; 0024-0047
(2019/04/04)
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- A paraquat emetic and preparation method
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The invention relates to the field of organic synthetic technology, in particular to a paraquat emetic and preparation method, comprises the following preparation steps, S1, preparation of [...]; S2, the preparation of the etherification; S3, pyrimidine triazole; S4, PP796 preparation. The invention one-pot method for directly simple high yield of synthetic method is more suitable for industrial production technology, the process route and is simple, low cost, production and operation method is simple and convenient, high yield, the total yield to methacrylic acid methyl ester idea can reach 43.5% or more, the obtained product and luster is pure white, crystalline state is good, content ≥ 99%.
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Paragraph 0018-0040; 0042
(2019/04/04)
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- Preparation method of paraquat vomitive, namely triazole pyrimidone
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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.
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Paragraph 0028; 0029; 0030; 0031; 0032; 0033; 0034-0044
(2018/03/28)
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- Process for preparing triazolopyrimidine derivatives
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A novel synthesis of triazolopyrimidine derivatives via the diamino-1,2,4-triazole is more efficient, cheaper and selective compared with existing syntheses.
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Page/Page column 7
(2008/06/13)
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- Process for preparing triazolopyrimidine derivatives
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A process for preparing triazolopyrimidine derivatives of the formula (I): wherein R1represents a hydrogen or an alkyl radical of one to ten carbon atoms, or a cycloalkyl radical of three to six carbon atoms, or an alkenyl radical of up to four carbon atoms; R2represents a hydrogen, a halogen atom, a hydroxyalkyl or alkyl radical of one to ten carbon atoms; R3represents a hydrogen, a hydroxyalkyl or alkyl radical of one to four carbon atoms; by rapidly preparing diamino-1,2,4-triazole which is reacted with an aldehyde to form an imide which is reacted with an α,β-unsaturated acid derivative, the reaction product of which is hydrolyzed in the presence of an acid to produce the triazolopyrimidine derivatives of formula (I). The compounds of the formula (I) are capable of preventing bronchospasm.
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