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Method for industrially producing butoconazole nitrate intermediate

A kind of technology of butconazole nitrate and intermediate, which is applied in the production field of 1-chloro-4--2-butanol as the intermediate of butconazole nitrate, and can solve the complex production process of butconazole nitrate, product yield and purity. It can not meet the problems of industrial production and high cost, and achieve the effect of being suitable for large-scale industrial production, reasonable raw materials and dosage, and easy operation.

Inactive Publication Date: 2015-12-30
ZHUZHOU QIANJIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented process simplifies its operation while reducing risks associated with handling dangerous chemicals or reagents used during manufacturing processes. It also results in higher yields and purification levels compared to previous methods that resulted in more unwanted substances being generated. Additionally it ensures consistently good products over time without any issues like contamination from other compounds produced along side.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving the efficiency or quality of producing butooconazoles that are effective treatments against vaginismus caused by yeast Candida albicans. Current methods require expensive equipment and produce impurities with poor yields and purification levels.

Method used

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  • Method for industrially producing butoconazole nitrate intermediate
  • Method for industrially producing butoconazole nitrate intermediate
  • Method for industrially producing butoconazole nitrate intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Prepare butoconazole nitrate intermediate 1-chloro-4-(4-chlorophenyl)-2-butanol as follows:

[0038] (1) Get 2.5kg of magnesium powder, 50ml of ether and a catalytic amount of iodine, add 40kg of p-chlorobenzyl ether solution with a concentration of 0.28g / ml dropwise at a rate of 3ml / s at 35°C, and after the dripping, add it at 38°C React for 1 hour to obtain p-chlorobenzyl Grignard reagent; then slowly add 20 kg of epichlorohydrin ether solution with a concentration of 0.35 g / ml dropwise, and react at 38° C. for 1.5 hours after dropping to obtain a reaction solution;

[0039] (2) Take the reaction solution obtained in step (1), add the sulfuric acid with a concentration of 25% dropwise at a rate of 2ml / s at 4°C under constant stirring, and stop the dripping when there is no solid residue; leave standstill after stirring at a constant speed for 10min The liquid was separated for 10 minutes; the aqueous phase was discarded, and the organic phase was concentrated at -0.01...

Embodiment 2

[0042] Compared with Example 1, the difference is only that the step (2) is specifically:

[0043] Get the reaction solution gained in step (1), add the sulfuric acid with a concentration of 24% dropwise at a rate of 1ml / s at 0°C under constant stirring, stop the dropwise addition when there is no solid residue; leave standstill for 8 minutes after stirring at a constant speed for 5 minutes to make the liquid Separate the layers; discard the water phase, take the organic phase and concentrate it at -0.05MPa, 50°C until no diethyl ether evaporates, collect the fraction at 160-180°C / 10mmHg by rectification, dry it, and obtain it.

[0044] The yield of the product of this embodiment is 77.4%.

[0045] After testing, the content of the target product 1-chloro-4-(4-chlorophenyl)-2-butanol is 90.27%, the content of p-chlorotoluene is 5.53%, and the content of chloromethylbenzene is 0.41%, 1, The content of 2-(4-chlorophenyl)ethane is 1.83%, the content of 1-chloro-4-(4-(chloro)benz...

Embodiment 3

[0047] Compared with Example 1, the difference is only that the step (2) is specifically:

[0048] (2) Get the reaction solution obtained in step (1), add the sulfuric acid with a concentration of 26% dropwise at a rate of 3ml / s at 10°C under constant stirring, and stop the dripping when there is no solid residue; leave standstill after stirring at a constant speed for 15min The liquid was separated for 12 minutes; the water phase was discarded, and the organic phase was concentrated at 0 MPa and 60°C until no ether evaporated, and the fraction at 160-180°C / 10mmHg was collected by rectification, and dried to obtain the product.

[0049] The yield of the product of this embodiment is 73.3%.

[0050] After testing, the content of the target product 1-chloro-4-(4-chlorophenyl)-2-butanol is 85.14%, the content of p-chlorotoluene is 10.47%, and the content of chloromethylbenzene is 0.43%, 1, The content of 2-(4-chlorophenyl)ethane was 1.81%, the content of 1-chloro-4-(4-(chloro)be...

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Abstract

The invention relates to a method for industrially producing a butoconazole nitrate intermediate 1-chloro-4-(4-chlorphenyl)-2-butanol. The method comprises the following steps: (1) taking magnesium powder and p-chlorobenzyl chloride as raw materials and iodine as a catalyst to prepare a p-chlorobenzyl chloride Grignard reagent in diethyl ether, and mixing the obtained p-chlorobenzyl chloride Grignard reagent with a diethyl ether solution of epichlorohydrin to fully react to obtain a reaction liquid; and (2) taking the reaction liquid obtained in the step (1), slowly dropwise adding sulfuric acid with concentration of 20-30% under the condition of an ice bath, stopping dropwise adding when no solid residues exist, standing for layering, discarding a water phase and concentrating and rectifying an organic phase, 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 optimizing the technological process, saving the raw materials and the time cost and increasing the purity and yield of the product. Therefore, the method is more suitable for large-scale industrial production.

Description

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Claims

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Application Information

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Owner ZHUZHOU QIANJIN PHARMA
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