4480-47-1Relevant articles and documents
Yanagihara et al.
, p. 554,555,556 (1972)
Novel synthesis method of metribuzin intermediate
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, (2020/01/25)
The invention discloses a novel synthesis method of a metribuzin intermediate, wherein the intermediate triazinone of metribuzin is produced by using pinacolone (methyl tert-butyl ketone) as an initial raw material through reaction steps of chlorination, hydrolysis, oxidation, condensation and the like. According to the invention, the reaction conditions are mild, and the total yield reaches 92.4%; hydrogen peroxide is used as an oxidizing agent for replacing sodium hypochlorite, and the oxidation reaction is carried out at a room temperature, so that the operation is convenient, and the byproduct is water so as to avoid the discharge of pollutants such as salt-containing wastewater and the like in the production process; and after the reaction is finished, the intermediate and the catalyst are subjected to chromatographic separation so as to recycle the water phase containing the catalyst.
Method for synthesizing tetra-2,3-(5-t-tutylpyrazine)metalloporphyrin
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Paragraph 0048; 0049; 0052; 0053; 0056; 0057, (2017/07/22)
The invention relates to a method for synthesizing tetra-2,3-(5-t-tutylpyrazine)metalloporphyrin. The method comprises the following steps: using 3,3-dimethyl-2-butanone as a raw material, carrying out a selenizing reaction with selenium dioxide, and rectifying the product to obtain 3,3-dimethyl-2-oxobutryaldehyde; heating 3,3-dimethyl-2-oxobutryaldehyde obtained in the above step in the condition that 2,3-diamido-2-2-butene dinitrile, urea and metal chloride exist, and purifying the product to obtain the tetra-2,3-(5-t-tutylpyrazine)metalloporphyrin. According to the method, the tetra-2,3-(5-t-tutylpyrazine)metalloporphyrin can be obtained only through a two-step reaction of selenylation and synthesis and then through simple purification, the process is simple, and the product is controllable; the used raw materials are simple, and the cost is low; no poisonous or harmful waste product is produced in the middle process, so that the process of after-treatment is greatly reduced. The tetra-2,3-(5-t-tutylpyrazine)metalloporphyrin prepared in the invention is high in yield.