67085-11-4Relevant articles and documents
A industrialized production butoconazole nitrate intermediates
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Paragraph 0069-0071, (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.
Butoconazole nitrate industrial production method
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Paragraph 0100-0103, (2018/05/16)
The invention relates to a method for industrially producing butoconazole nitrate. The method comprises the following steps: (1) taking 1-8 parts of 1-(2-chloro-4-(4-chlorphenyl)butyl)-1-hydro-imidazole, 1-8 parts of 2,6-dichlorothiophenol, 1-5 parts of anhydrous potassium carbonate and 30-50 parts of acetone to undergo heating reflux reaction for 4-6 hours, then replenishing 0.1-1 part of anhydrous potassium carbonate, continuously carrying out heating reflux reaction for 5-9 hours, cooling and filtering the reactant and concentrating the filtrate, thus obtaining a concentrate; (2) taking the concentrate obtained in the step (1), adding extract liquor formed by an organic solvent and water, and after full extraction, retaining an organic phase for later use; (3) dropwise adding concentrated nitric acid to the organic phase obtained in the step (2) and carrying out filtration after stopping generating a precipitate; discarding the filtrate and washing and drying a filter cake, thus obtaining butoconazole nitrate. In the method provided by the invention, the conditions and parameters in the synthetic process are comprehensively and preferentially selected, and the impurities which are likely to be introduced in the production process are effectively controlled, thus increasing the production efficiency and the purity and yield of the product. Therefore, the method is more suitable for large-scale industrial production.
Butoconazole nitrate industrial production method
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Paragraph 0107; 0108; 0109, (2018/05/24)
The invention relates to a method for producing butoconazole nitrate. The method comprises the following steps: (1) taking 1-(2-chloro-4-(4-chlorphenyl)butyl)-1-hydro-imidazole, 2,6-dichlorothiophenol and anhydrous potassium carbonate as raw materials to undergo heating reflux in acetone, after full reaction, cooling and filtering the reactant and concentrating the filtrate, thus obtaining a concentrate; (2) taking the concentrate obtained in the step (1) and adding extract liquor which comprises diethyl ether and water in a weight ratio of (2-3) to (1-2); after full extraction, discarding a water phase and retaining an organic phase for later use; (3) dropwise adding concentrated nitric acid to the organic phase obtained in the step (2) and carrying out filtration after stopping generating a precipitate; discarding the filtrate and washing and drying a filter cake, thus obtaining butoconazole nitrate. In the method provided by the invention, the conditions and parameters in the synthetic process are comprehensively and preferentially selected, and the impurities which are likely to be introduced in the production process are effectively controlled, thus increasing the production efficiency and the purity and yield of the product. Therefore, the method is more suitable for large-scale industrial production.
