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Preparation method of prothioconazole I-type crystal form

A technology of prothioconazole and crystal form, which is applied in the field of preparation of prothioconazole type I crystal form, can solve the problems of low product yield, poor stability, cumbersome operation, etc., and achieve high purity and crystal form Regular and simple operation steps

Pending Publication Date: 2020-04-10
HAILIR PESTICIDES & CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the disadvantages of serious solvent residue, cumbersome operation, low product yield, low purity and poor stability in the method for preparing prothioconazole type I crystal form in the prior art. The technical scheme of the present invention is based on Isopropanol or a mixture of isopropyl ether and ethanol is used as a solvent, and the prothioconazole type II crystal form can be prepared quickly, effectively and simply by cooling method. The product has no solvent residue, easy operation, high yield, high purity, Good stability, not easy to coalesce, suitable for industrial production

Method used

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  • Preparation method of prothioconazole I-type crystal form
  • Preparation method of prothioconazole I-type crystal form
  • Preparation method of prothioconazole I-type crystal form

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A preparation method of prothioconazole type I crystal form, the specific steps are as follows:

[0028] Put 0.344 g of prothioconazole crude drug in a round bottom flask, add 3ml of toluene into the round bottom flask, heat and stir in a water bath at 50°C for 3 hours, filter while hot, and let the filtrate stand for 3 days after cooling to room temperature to collect the precipitated solid The phase was subjected to negative pressure suction filtration to obtain 0.325 g of type I prothioconazole crystals, the content detected by HPLC analysis: 99.9%, and the melting range: 140.1-140.4°C. The main particle size is 180μm, the bulk density is 0.58g / mL, and the angle of repose is 30°. Use D8 X-ray diffractometer of German BRUKER company to measure, the test conditions are Cu-Kα target tube voltage 40kV, tube current 10mA, scan speed 2° / min, the PXRD diffraction pattern of the product can be found in figure 1 , based on the characteristic reflection, it was confirmed to b...

Embodiment 2

[0030] A preparation method of prothioconazole type I crystal form, the specific steps are as follows:

[0031] Put 0.344 g of a mixture of prothioconazole type I crystals and type II crystals (mass ratio: 2:8) in a round bottom flask, add 3 ml of toluene into the round bottom flask, heat and stir in a water bath at 60°C for 2 hours, and filter while hot , the filtrate was cooled to room temperature and then left to stand for 4 days to collect the precipitated solid phase, and filtered under negative pressure to obtain 0.338 g of type I prothioconazole crystals, the content of which was detected by HPLC analysis: 99.9%, and the melting range: 140.1-140.3°C. The main particle size is 180μm, the bulk density is 0.58g / mL, and the angle of repose is 30°. The spectrum of the product was obtained after PXRD detection, and based on the characteristic reflection, it was confirmed to be the crystal form of prothioconazole I.

Embodiment 3

[0033] A preparation method of prothioconazole type I crystal form, the specific steps are as follows:

[0034]Put 0.344 g of amorphous prothioconazole in a round-bottomed flask, add 3 ml of toluene into the round-bottomed flask, heat and stir in a water bath at 80°C for 2 hours, filter while hot, and let the filtrate stand for 4 days after cooling to room temperature to collect the precipitated The solid phase was filtered under negative pressure to obtain 0.338 g of type I prothioconazole crystals, the content detected by HPLC analysis: 99.9%, and the melting range: 140.0-140.5°C. The main particle size is 180μm, the bulk density is 0.58g / mL, and the angle of repose is 30°. The spectrum of the product was obtained after PXRD detection, and based on the characteristic reflection, it was confirmed to be the crystal form of prothioconazole I.

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Abstract

The invention relates to the field of compound crystal forms, in particular to a preparation method of a prothioconazole I-type crystal form. The preparation method comprises the following steps: dissolving a prothioconazole raw material in a solvent, filtering to obtain filtrate, standing the filtrate and separating out a solid phase, namely the prothioconazole I-type crystal form. According to the technical scheme, the prothioconazole I-type crystal form is prepared through a solvent evaporation method and a cooling method, the method is simple and easy to implement and low in cost, and theprepared product is high in yield and purity, good in stability without coalescence and suitable for being applied to industrial production.

Description

technical field [0001] The invention belongs to the field of compound crystal forms, and in particular relates to a preparation method of prothioconazole type I crystal form. Background technique [0002] Prothioconazole is a new type of broad-spectrum triazolethione fungicide developed by Bayer Corporation of Germany. Since its launch, prothioconazole has been highly valued by the industry. In 2015, the global sales of prothioconazole exceeded US$800 million, ranking third in the global sales of fungicides. Prothioconazole is mainly used for the control of cereals, wheat and legumes. [0003] With the gradual deepening of drug research and development, the study of drug crystal forms has also become the focus of drug researchers. According to different research reports, the crystal form of a drug has a major impact on the physical and chemical properties of the drug, thus profoundly affecting the actual use of the drug. Bayer company discloses the method for recrystalliz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/12
CPCC07D249/12C07B2200/13
Inventor 葛家成白光耀王旭李建国王凯
Owner HAILIR PESTICIDES & CHEM GRP
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