64211-06-9Relevant articles and documents
Synthesis process of high-purity oxiconazole nitrate
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Paragraph 0047-0049; 0055-0057; 0059-0060; 0063-0065; ..., (2021/09/15)
The invention relates to a synthesis process of high-purity oxiconazole nitrate, and belongs to the technical field of pharmacy, thesynthesis process comprises the following steps: 1, stirring and mixing 2-chloro-1-(2, 4-dichlorophenyl) ethanone, imidazole and absolute methanol, carrying out reflux reaction, adding hydrogen peroxide, ammonia monohydrate and a modified catalyst, continuously reacting, and purifying, and obtaining (Z)-2 '-(1H-imidazole-1-yl)-2, 4-dichloroacetophenone oxime with relatively high purity; 2, (Z)-2 '-(1H-imidazole-1-yl)-2, 4-dichloroacetophenone oxime and 2, 4-dichlorobenzyl chloride are subjected to a substitution reaction, high-purity oxiconazole nitrate is obtained through suction filtration, washing, drying and recrystallization, the traditional synthesis process is analyzed, the synthesis method and the mode of adding a modified catalyst are changed, generation of impurities is reduced, the purity of products in production links is improved, the synthesis steps are reduced, the synthesis route is shortened and the production efficiency is improved.
Process for the stereospecific preparation of (Z)-1-(2,4-dichlorophenyl)-2-(imidazol-1-yl)-0-(2,4-dichlorobenzyl)-ethanone oxime ether
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, (2008/06/13)
For preparing substantially pure (Z)-1-(2,4-dichlorophenyl)-2-(imidazol-1-yl)-0-(2,4-dichlorobenzyl)-ethanone oxime ether having the formula STR1 i.e. the cis-isomer of said oxime ether in a stereospecifically pure form, the pure (Z)-stereoisomer of the corresponding ethanone oxime is first converted into an alkali salt in a polar solvent, such as acetone or dimethylformamide, using an alkali in an amount somewhat less than the equimolar amount with respect to the said ethanone oxime, and is then converted to the desired ether by reacting it at a temperature not higher than 40° C. with a halogen compound capable of forming the desired ether. Isolation of the ether product is obtained as the free base or by precipitating it as an acid addition salt upon addition of a suitable organic or mineral acid, preferably nitric acid.