A kind of preparation method of 4-amino-2,6-dimethoxypyrimidine

A technology of dimethoxypyrimidine and hydroxypyrimidine sodium salt is applied in the field of preparation of 4-amino-2,6-dimethoxypyrimidine, and can solve the problems of hidden dangers in production safety, aggravated by-products, high pressure on environmental protection and the like, Achieve the effect of reducing equipment requirements, simple equipment, and reducing pollutant emissions

Inactive Publication Date: 2018-05-29
滨海新东方医化有限公司
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AI Technical Summary

Problems solved by technology

This method chlorination process uses excessive phosphorus oxychloride as chlorination reagent and solvent, and excessive phosphorus oxychloride not only can aggravate the generation of by-product 4-amino-2,6-dichloropyrimidine phosphorus oxychloride, and It is easy to explode when exposed to water, which brings safety hazards to production
In addition, what is even more unfavorable is that the process of acidification and chlorination will produce a large amount of colored, strongly acidic, salt-containing, and phosphorus-containing wastewater (about 35-40 tons of wastewater generated per ton of product), and the pressure on environmental protection is great.

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  • A kind of preparation method of 4-amino-2,6-dimethoxypyrimidine
  • A kind of preparation method of 4-amino-2,6-dimethoxypyrimidine

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specific Embodiment approach

[0008] 1. The process is simple and the equipment is simple. The acidification and chlorination processes in the traditional process are omitted, and the finished product can be obtained only in two steps of cyclization and methylation. And all reactions can be carried out in the same vessel, reducing equipment requirements. 2. The yield has been greatly improved. Because 4-amino-2,6-dihydroxypyrimidine sodium salt is easy to open and hydrolyze in water, the yield of the original process is not high. The 4-amino-2,6-dihydroxypyrimidine sodium salt generated by the present invention does not need to be separated, and can directly participate in the next step reaction, thereby avoiding its ring-opening hydrolysis. 3. The chlorination process is omitted, the production cost is reduced, and the operating environment is greatly improved. 4. Significantly reduce pollutant emissions. The acidification, chlorination and methoxylation processes in the original process all produce a...

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Abstract

The invention relates to an organic synthesis method, in particular to a preparation method of 4-amino-2,6-dimethoxypyrimidine. According to the method, 4-amino-2,6-dihydroxypyrimidine sodium salt is prepared from methyl cyanoacetate, urea and sodium methylate as raw materials through cyclization; then 4-amino-2,6-dimethoxypyrimidine is prepared with a one-pot process through methylation of dimethyl sulfate. The preparation method has the advantages that a process route is simplified, reaction conditions are improved, the product quality is improved, the product yield is increased, three wastes are reduced substantially, and a green and feasible scheme is provided for industrial production.

Description

technical field [0001] The invention relates to a preparation method of 4-amino-2,6-dimethoxypyrimidine, and belongs to the field of chemical synthesis. Background technique [0002] The existing method of synthesizing 4-amino-2,6-dimethoxypyrimidine has following two kinds: [0003] One is to use barbituric acid as raw material, first chlorinate with phosphorus oxychloride to generate trichloropyrimidine, and then conduct ammoniation to obtain 4-amino-2,6-dichloropyrimidine and 2-amino-4,6- Dichloropyrimidine, the former accounts for about 1 / 3 and the latter accounts for about 2 / 3. After separation, methoxylation is performed to obtain 4-amino-2,6-dimethoxypyrimidine; The product was directly methoxylated and isolated. The intermediate trichloropyrimidine produced by this method is highly toxic, and generates a large number of isomers, which is difficult to separate and has a low total yield. Second, 4-amino-2,6-dihydroxypyrimidine sodium salt is prepared by cyclization ...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52
CPCC07D239/52
Inventor 缪宗德
Owner 滨海新东方医化有限公司
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