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Triazole sulcotrione polymorph B, preparation method thereof and application

A technology of fensulfotrione and crystal form, which is applied in the field of herbicide crystallization technology, and can solve the problem of no crystal form, etc.

Active Publication Date: 2017-08-11
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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  • Triazole sulcotrione polymorph B, preparation method thereof and application
  • Triazole sulcotrione polymorph B, preparation method thereof and application
  • Triazole sulcotrione polymorph B, preparation method thereof and application

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 3,000 grams of triazosulfotrione A crystal form technical substance in a 10L flask, add 6L of dichloromethane, heat and stir until the raw materials are completely dissolved, stop heating after the raw materials are completely dissolved, gradually lower the temperature to about 10°C, and let stand After 1 hour, filter, and dry at 15° C. under normal pressure for 5 hours to obtain triazosulfotrione B crystal powder. It can also be naturally volatilized at 25°C until the dichloromethane is completely volatilized to obtain triazosulfotrione B crystal powder.

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Abstract

The invention belongs to the technical field of herbicide crystallization processes, and particularly relates to triazole sulcotrione polymorph B, a preparation method thereof and an application. An X-ray powder diffraction pattern of the triazole sulcotrione polymorph B has characteristic peaks when diffraction angles 2-theta are 7.1 degrees, 7.3 degrees, 9.6 degrees, 11.8 degrees, 13.4 degrees, 14.2 degrees, 14.6 degrees, 14.9 degrees, 18.2 degrees, 18.8 degrees, 19.1 degrees, 19.6 degrees, 19.9 degrees, 21.0 degrees, 21.4 degrees, 21.7 degrees, 22.6 degrees, 24.1 degrees, 24.4 degrees, 25.1 degrees, 25.8 degrees, 26.4 degrees, 27.2 degrees, 27.7 degrees, 28.0 degrees, 28.6 degrees, 29.4 degrees, 32.1 degrees, 34.7 degrees, 35.9 degrees, 36.8 degrees, 38.8 degrees, 39.3 degrees and 39.7 degrees. The triazole sulcotrione polymorph B is good in stability, the polymorph B or a compound composition of the polymorph B and other effective components has good control effect on gramineous weeds of rice fields and parts of broadleaf weeds, and the control effect of the polymorph B is obviously superior to that of polymorph A.

Description

technical field [0001] The invention belongs to the technical field of herbicide crystallization technology, and in particular relates to a crystal form B 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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IPC IPC(8): C07D231/20A01N43/56A01P13/00
CPCA01N43/56C07B2200/13C07D231/20A01N2300/00
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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