250593-00-1Relevant articles and documents
Method for recycling byproducts in synthesis of diphenyl sulfide compound
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Paragraph 0099; 0103-0105, (2021/03/30)
The invention provides a method for recycling byproducts in synthesis of a diphenyl sulfide compound. The byproducts comprise alkyl alcohol and dimethyl disulfide. The method comprises the steps of (1) mixing the byproducts in synthesis of the diphenyl sulfide compound with a sodium nitrite aqueous solution, adding concentrated hydrochloric acid for reaction, and obtaining alkyl nitrite and dimethyl disulfide; and (2) mixing the products obtained in the step (1) with copper powder, adding an aniline compound for reaction, carrying out desolvation treatment on the obtained reaction solution toobtain a diphenyl sulfide compound and byproducts, and returning the byproducts to the step (1). According to the recycling method, the byproducts do not need to be separated, the byproducts serve asraw materials to be directly applied to synthesis of the diphenyl sulfide compound, the process steps are simple and safe, cyclic utilization of the materials is achieved, and the raw material cost ofindustrial production of the diphenyl sulfide compound and the treatment cost of industrial three wastes are remarkably reduced.
Topramezone intermediate and topramezone preparation method
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Paragraph 0073-0075, (2020/04/06)
The invention relates to the field of organic synthesis, in particular to a topramezone intermediate and a topramezone preparation method. The topramezone preparation method comprises the following steps: 3-[3-halogen-2-methyl-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole and cyanide are subjected to a substitution reaction to obtain 3-[3-cyano-2-methyl-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole; hydrolysis reaction is performed on 3-[3-cyano-2-methyl-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole under the action of acid or alkali to obtain 2-methyl-3-(4, 5-dihydroisoxazole-3-yl)-4-methylsulfonyl benzoic acid; and 2-methyl-3-(4, 5-dihydroisoxazole-3-yl)-4-methylsulfonyl benzoic acid and 1-methyl-5-hydroxypyrazole are condensed and rearranged to generate topramezone. According to the topramezone intermediate and the topramezone preparation method provided by the invention, the use of an expensive palladium catalyst and a dangerous butyl lithium reagent is avoided, the yield isrelatively high, the cost is reduced, the process is simplified, the defects in the prior art are overcome, and the industrial value is achieved.
Synthesis method and application of topramezone impurity
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, (2019/10/01)
The invention discloses a synthesis method of topramezone impurity. The method includes: taking 2, 3-dimethylaniline as the starting raw material, carrying out methyl sulfidation, bromination, oxidation, oximation and chlorination ring-closing to synthesize 3-[3-bromo-2-methyl-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole, and carrying out condensation with 1-methyl-5-hydroxypyrazole under an alkaline condition to synthesize 3-[2-methyl-3-(1-methyl-1H-pyrazole-5-oxyl)-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole. The invention also discloses application of the corresponding product. The synthesis method provided by the invention has the characteristics of simple operation, easily control process, and a product yield of 40%-80%. The obtained product can be used as a standard substancefor detecting and monitoring the synthesis of topramezone.
The Synthesis and Crystal Structure of a Novel Pesticide Intermediates
He, Zhipeng,Ren, Tiegang,Li, Yongzhe,Fang, Xiaomin
, p. 419 - 426 (2015/10/12)
A novel pesticide intermediates 3-(6-bromo-2-methyl-3-(methylsulfonyl)phenyl)-4,5-dihydroisoxazole was synthesized with 2,3-dimethylaniline as the starting materials. The final product and intermediates were characterized by mass spectra, 1H NMR, infrared and elemental analysis. The crystal structure of compounds 6 and 8 were determined by single crystal X-ray diffraction. Results shown that two oxazole compounds crystallize in the monoclinic (6) and triclinic (8) with the space group of P 21/c for 6 and P-1 for 8, respectively.
Method and novel intermediate products for producing isoxazolin-3-yl-acylbenzenenes
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, (2008/06/13)
The present invention describes a process for preparing isoxazoles of the formula I where: R1is hydrogen, C1-C6-alkyl, R2is hydrogen, C1-C6-alkyl, R3, R4, R5are each hydrogen, C1-C6-alkyl or R4and R5together from a bond, R6is a heterocysclic ring, n is 0, 1 or 2; which comprises preparing an intermediate of the formula VI where R1, R3, R4and R5are each as defined above, followed by halogenation, thiomethylation, oxidation and acylation to give compounds of the formula I. Furthermore, the invention describes novel intermediates for preparing the compounds of the formula I and novel processes for preparing the intermediates.
