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Nicosulfuron crystal form and preparation method thereof

The technology of nicosulfuron-methyl crystal and nicosulfuron-methyl is applied in the field of nicosulfuron-methyl crystal form and its preparation, which can solve the problems of easy coalescence, poor fluidity and the like, and achieves good repeatability, good growth and good stability Effect

Active Publication Date: 2018-07-20
内蒙古新农基科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In order to overcome the deficiencies of the prior art and solve the problems of poor fluidity and easy aggregation of existing products of nicosulfuron, the application provides a nicosulfuron crystal form and a preparation method thereof

Method used

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  • Nicosulfuron crystal form and preparation method thereof
  • Nicosulfuron crystal form and preparation method thereof
  • Nicosulfuron crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 2.4g of nicosulfuron in 20g of ethanol solvent, stir at 40°C for suspension crystallization, filter while hot after 40h to obtain white crystals, dry at 20°C for 12h to obtain nicosulfuron crystals. The powder X-ray diffraction pattern of the product is represented by diffraction angle 2θ at 10.0, 11.3, 12.0, 13.24, 15.5, 16.6, 19.3, 19.7, 20.0, 21.7, 22.7, 23.8, 24.1, 24.6, 25.1, 26.4, 26.7, 26.9 , 27.8, 28.4, 29.4, 30.1, 31.3, 32.8, 33.2, 34.3, 35.2, 36.4, 37.1, 37.8, 38.9, 39.3 degrees have characteristic peaks, and figure 1 Consistent, the DSC spectrum has a characteristic endothermic peak at 187 ° C, which is consistent with figure 2 consistent, confirming that the obtained product is the Nicosulfuron-methyl Form III crystal. The crystals are massive, with Figure 4 Similarly, it has a bulk density of 0.6411 g / ml and an angle of repose of 24°.

Embodiment 2

[0027] Put 3 g of nicosulfuron in 20 g of ethanol solvent, stir at 40°C for suspension crystallization, filter while hot after 40 hours to obtain white crystals, dry at 40°C for 6 hours to obtain nicosulfuron crystals. The powder X-ray diffraction pattern of the product is represented by diffraction angle 2θ at 10.1, 11.4, 12.1, 13.3, 15.5, 16.7, 19.3, 19.8, 20.1, 21.8, 22.8, 23.9, 24.2, 24.7, 25.2, 26.5, 26.8, 26.9 , 27.9, 28.5, 29.5, 30.2, 31.4, 32.9, 33.3, 34.4, 35.3, 36.5, 37.2, 37.9, 38.9, 39.4 degrees have characteristic peaks, and figure 1 Consistent, the DSC spectrum has a characteristic endothermic peak at 188 ° C, which is consistent with figure 2 consistent, confirming that the obtained product is the Nicosulfuron-methyl Form III crystal. The crystals are massive, with Figure 4 Similarly, it has a bulk density of 0.6420 g / m and an angle of repose of 24°.

Embodiment 3

[0029]Put 3.4g of nicosulfuron in 20g of ethanol solvent, stir at 40°C for suspension crystallization, filter while hot after 48h to obtain white crystals, dry at 30°C for 10h to obtain nicosulfuron crystals. The powder X-ray diffraction pattern of the product is represented by diffraction angle 2θ at 10.0, 11.3, 12.0, 13.24, 15.5, 16.6, 19.3, 19.7, 20.0, 21.7, 22.7, 23.8, 24.1, 24.6, 25.1, 26.4, 26.7, 26.9 , 27.8, 28.4, 29.4, 30.1, 31.3, 32.8, 33.2, 34.3, 35.2, 36.4, 37.1, 37.8, 38.9, 39.3 degrees have characteristic peaks, and figure 1 Consistent, the DSC spectrum has a characteristic endothermic peak at 186 ° C, which is consistent with figure 2 consistent, confirming that the obtained product is the Nicosulfuron-methyl Form III crystal. The crystals are massive, with Figure 4 Similarly, it has a bulk density of 0.6420 g / ml and an angle of repose of 25°.

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Abstract

The invention relates to a nicosulfuron crystal form and a preparation method thereof. A characteristic endothermic peak at 187 + / - 2 DEG C exists in the DSC map of the nicosulfuron crystal form. Themethod adopts a constant temperature suspension crystal transformation technology, and concretely comprises the following steps: adding crude nicosulfuron to ethanol according to a mass ratio of nicosulfuron to the solvent ethanol of 0.12-0.17, stirring the nicosulfuron and ethanol at a constant temperature suspension crystal transformation temperature of 40-50 DEG C for 36-48 h to generate a white solid, filtering the obtained product while hot, and drying the filtered product to obtain the nicosulfuron crystal. The product is a well-growth block crystal, has a good fluidity, is not prone tocoalesce, has a high bulk density reaching 0.6421 g / ml, and has an angle of repose of 24 DEG, and the method is beneficial to the preparation production, filtration and other operations, and solves the problems of easiness in coalescence and difficulty in preparation production of existing acicular crystals.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical crystallization, and in particular relates to a nicosulfuron crystal form and a preparation method thereof. Background technique [0002] Nicosulfuron was first discovered as a sulfonylurea systemic herbicide by Ishihara Sangyo Co., Ltd. in Japan. In the late 1980s, Ishihara Sangyo Co., Ltd. and DuPont Company of the United States jointly developed it and officially put it into use as a cornfield herbicide. use. It can be absorbed by the stems, leaves and roots of weeds, and then conducts in the plant body, causing sensitive plants to stagnate, chlorotic stems and leaves, and gradually wither. Generally, they die within 20-25 days, but in the case of low temperature, it is harmful to certain plants. Some perennial weeds take longer. The efficacy of pesticide application is good before the 4-leaf stage after budding, and the efficacy of pesticide application decreases when the seedlings ar...

Claims

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Application Information

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IPC IPC(8): C07D401/12
CPCC07B2200/13C07D401/12
Inventor 龚俊波刘裕王静康尹秋响侯宝红吴送姑姜爽贾丽娜
Owner 内蒙古新农基科技有限公司
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