51135-73-0Relevant articles and documents
Preparation method of (by machine translation)
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Paragraph 0039, (2020/06/24)
The invention relates to a novel process for preparing flutamipide by using a pharmaceutical active pharmaceutical ingredient, wherein ethyl acetoacetate is taken as a raw material and mixed with hydroxylamine hydrochloride to obtain fluticide. The process not only can better control the content of 3 - methyl isomers and 4 - trifluoromethylaniline in the baflunomide product, and is higher in yield and more concise. The industrial wastewater generated by the process is less in waste gas, environmentally friendly, capable of effectively reducing production cost and corrosion to equipment. (by machine translation)
Synthesis and fungicidal activities of 1-(5-Methylisoxazoyl-4-carbonyl)-4- arylsulfonyl thiosemicarbazides
Ye, Dong-Ju
scheme or table, p. 1503 - 1506 (2012/04/10)
1-(5-Methylisoxazoyl-4-carbonyl)-4-arylsulfonyl thiosemicarbazides, which were prepared by treatment of arylsulfonyl hydrazine with 5-methylisoxazole-4- carbonyl isothiocyanate in good yields. The structures of all compounds were confirmed by 1H NMR, MS and elemental analyses. The preliminary bioassays indicated that some compounds are comparable to the commercial fungicides. Some of these compounds also exhibit moderate fungicidal activities.
Process for preparing 5-methylisoxazole-4-carboxylic- (4'-trifluoromethyl)-anilide
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, (2008/06/13)
A process for preparing 5-methylisoxazole-4-carboxylic-(4′-trifluoromethyl)-anilide comprising: (a) reacting ethylacetoacetate, triethylorthoformate, and acetic anhydride at a temperature of from about 75° C. to about 150° C., to form ethyl ethoxymethyleneacetoacetic ester; (b) combining the ethyl ethoxymethyleneacetoacetic ester with sodium acetate or a salt of trifluoroacetic acid in the presence of hydroxylamine sulfate at a temperature of from about ?20° C. to 10° C., to form ethyl-5-methylisoxazole-4-carboxylate; (c) reacting the ethyl-5-methylisoxazole-4-carboxylate with a strong acid to form 5-methylisoxazole-4-carboxylic acid; (d) reacting the crystallized 5-methylisoxazole-4-carboxylic acid with thionyl chloride to form 5-methylisoxazole-4-carbonyl chloride; and (e) reacting the 5-methylisoxazole-4-carbonyl chloride with trifluoromethyl aniline and an amine base at a temperature of from about 0° C. to about 50° C. to form 5-methylisoxazole-4-carboxylic-(4′-trifluoromethyl)-anilide. The process of the invention is especially advantageous for preparing 5-methylisoxazole-4-carboxylic-(4′-trifluoromethyl)-anilide, since the process: (1) eliminates or reduces the formation of the by-product 2-cyanoacetoacetic-1-(4′-trifluoromethyl)-anilide (CATA), generally as low as 0.0006%; (2) eliminates or reduces the formation of isomeric impurity ethyl-3-methyisoxazole-4-carboxylate and its corresponding acid as low as 0.1%, (3) produces a high quality of 5-methylisoxazole-4-carboxylic-(4′-trifluoromethyl)-anilide generally having 99.8-100% HPLC potency; and (4) does not require distillation of the isoxazole ester.