67085-12-5Relevant articles and documents
A industrialized production butoconazole nitrate intermediates
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Paragraph 0007; 0050-0054; 0057-0058; 0061-0062; 0064-0065, (2018/05/24)
The invention relates to a method for industrially producing a butoconazole nitrate intermediate 1-(2-chlorine-4-(4-chlorphenyl) butyl)-1hydrogen-imidazole. The method comprises steps as follows: (1), 2-5 parts of 1-(2-hydroxyl-4-(4-chlorphenyl) butyl)-1hydrogen-imidazole is taken and sufficiently dissolved in 20-40 parts of dichloromethane, 2-5 parts of thionyl chloride are slowly and dropwise added at the temperature of 15 DEG C-25 DEG C, the mixture is slowly heated to 25 DEG C-65 DEG C for a sufficient reaction and cooled, and a reaction liquid is obtained; (2), cold water and anhydrous sodium carbonate are sequentially and slowly added to the reaction liquid obtained in the step (1), suction filtration is performed, solids are abandoned, a liquid is concentrated and dried, and the butoconazole nitrate intermediate is obtained. According to the provided method, conditions and parameters in the synthesis process are comprehensively and preferentially selected, the purity and the yield of products are improved, and the method is more suitable for large-scale industrial production.
A industrialized production butoconazole nitrate intermediates
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Paragraph 0052-0054, (2018/05/24)
The invention relates to a method for industrially producing a butoconazole nitrate intermediate 1-(2-chloro-4-(4-chlorphenyl)butyl)-1-hydro-imidazole. The method comprises the following steps: (1) taking 1-(2-hydroxy-4-(4-chlorphenyl)butyl)-1-hydro-imidazole and thionyl chloride as raw materials to undergo heating reflux in dichloromethane, and after full reaction, cooling the reactant, thus obtaining a reaction liquid; and (2) slowly adding cold water and anhydrous sodium carbonate to the reaction liquid obtained in the step (1) in sequence, carrying out suction filtration, discarding the solid, concentrating the liquid and drying the concentrate, thus obtaining the butoconazole nitrate intermediate. In the method provided by the invention, the conditions and parameters in the synthetic process are comprehensively and preferentially selected, thus increasing the purity and yield of the product. Therefore, the method is more suitable for large-scale industrial production.
Preparation method of butoconazole nitrate
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Paragraph 0043; 0047; 0053; 0057, (2018/01/11)
The invention discloses a preparation method of butoconazole nitrate. The preparation method comprises the following steps: with 4-chlorobenzyl chloride as a starting raw material, synthesizing 1-chloro-4-(4-chlorophenyl)-2-butanol, then synthesizing 1-(4-(4-chlorophenyl)-2-hydroxy-butyl) imidazole, then synthesizing 1-(4-(4-chlorophenyl)-2-chloro-butyl) imidazole, adding the 1-(4-(4-chlorophenyl)-2-chloro-butyl) imidazole, 2, 6-dichlorobenzenethiol and potassium carbonate into acetone, heating for refluxing, adding water and ethyl acetate after the completion of a reaction, performing liquid separation, sequentially washing an ethyl acetate phase by using saturated potassium carbonate and saturated salt water, drying by using anhydrous magnesium sulfate, removing magnesium sulfate, dropwise adding nitric acid with the concentration of 65% in an ice bath until no precipitate is produced, filtering for collecting solid, and recrystallizing by using absolute ethanol to obtain white crystals, namely the butoconazole nitrate. By the preparation method of the butoconazole nitrate, the process is simple, the yield is high, the cost is low, and the purity of the obtained product is high.