Crystal form C of triazolesulcotrione and preparation method and application thereof

A technology of mesosulfatrione and its crystal form, which is applied in the field of herbicide crystallization technology, can solve the problems of no crystal form, etc., and achieve the effects of high solubility, high biological activity and good stability

Active Publication Date: 2017-07-14
QINGDAO KINGAGROOT CHEM COMPOUNDS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Since triazosulfotrione is a newly developed drug, there are no reports of its crystal form in various literatures and patents

Method used

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  • Crystal form C of triazolesulcotrione and preparation method and application thereof
  • Crystal form C of triazolesulcotrione and preparation method and application thereof
  • Crystal form C of triazolesulcotrione and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] According to the method of CN 105503728 B, the original drug of triazole sulfotrione is prepared. Then put 3000 grams of triazosulfotrione original drug in a 10L flask, add 5L of acetone, heat to 50°C, stir until the raw material is completely dissolved, cool down to 0°C, let stand for 2 hours, filter, 30°C normal pressure drum Air-dried for 5 hours to obtain triazole sulfotrione A crystal powder. Or the solvent is volatilized until the solvent is completely volatilized, and the powder of triazosulfotrione A crystal form can also be obtained.

Embodiment 2

[0041] Put 2000 grams of triazosulfotrione A crystal form technical substance in a 10L flask, add 5L of dichloromethane, heat and stir until the raw material is completely dissolved, gradually lower the temperature to about 10°C, let stand for 1 hour, and filter to obtain crystals. Then, it was dried at 110° C. for 1 hour to obtain crystal form C powder.

Embodiment 3

[0043]Put 2000 grams of triazosulfotrione A crystal form technical substance in a 10L flask, add 3L of ethyl acetate, 3L of ethanol and 1L of water, stir until the raw materials are completely dissolved, and then volatilize naturally until the solvent is completely volatilized to obtain triazole Powder of crystal form C of sulcotrione.

[0044] Physical and chemical stability experiment

[0045] The crystal form A of triazosulfotrione obtained in Example 1 and the crystal form C of triazole sulfotrione obtained in Examples 2 and 3 were used as powders, and the contents of crystal form A and two crystal forms C were both 95.0% by HPLC. %, after that, these three powders were placed in ovens at 25°C, 40°C, 55°C and 70°C respectively, and placed in an oven for 2 months for heat storage experiments, and then the crystal type and purity were tested. The results are shown in Table 1 below:

[0046] Table 1 Stability investigation of different crystal forms of triazosulfotrione

[...

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Abstract

The invention belongs to the technical field of crystallization processes of herbicides and in particular relates to a crystal form C of triazolesulcotrione and a preparation method and application thereof. The X-ray powder diffraction spectrogram of the crystal form C of triazolesulcotrione has characteristic peaks at diffraction angles 2theta of 6.8, 7.6, 9.4, 11.1, 13.1, 13.5, 14.6, 15.5, 16.1, 16.9, 18.0, 19.3, 19.4, 20.9, 21.9, 23.3, 23.6, 23.8, 24.8, 25.5, 26.1, 26.8, 27.8, 28.9, 30.1, 31.3, 33.2, 34.3 and 36.0, wherein the 2theta error range is within +/-0.2 degree. Through tests, the crystal form C of triazolesulcotrione provided by the invention is good in stability; the crystal form is not transformed after being stored for two months at a high temperature of 70 DEG C, the purity is substantially not reduced, and the solubility in water is increased by nearly one time; moreover, and a compound composition of the crystal form C or other active ingredients has a relatively good control effect on gramineous weeds and part of broadleaf weeds in paddy fields, which is obviously superior to that of a crystal form A.

Description

technical field [0001] The invention belongs to the technical field of herbicide crystallization technology, and in particular relates to a crystal form C of triazosulfotrione, a preparation method and application thereof. Background technique [0002] The chemical name of triazole sulfotrione: 4-(2-chloro-3-((3,5-dimethyl-1H-pyrazol-1-yl)methyl)-4-(methylsulfonyl)benzyl Acyl)-1,3-dimethyl-1H-pyrazol-5-yl-1,3-dimethyl-1H-pyrazole-4-carboxylate [0003] Structural formula: [0004] [0005] Triazole sulfotrione is a newly developed HPPD inhibitor herbicide for post-emergence stem and leaf treatment of rice fields. It has excellent biological activity and can effectively control a variety of malignant weeds in rice fields. The patent of the compound has been authorized. The authorized announcement number: CN105503728 B. [0006] Polymorphism refers to the phenomenon that solid substances form solid states with different physical and chemical properties in two or more dif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/20A01N43/56A01P13/00
CPCA01N43/56C07B2200/13C07D231/20
Inventor 赵德陈志祥林贝贝张兆真彭学岗张景远
Owner QINGDAO KINGAGROOT CHEM COMPOUNDS CO LTD
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