Crystal form of nicosulfuron and preparation method thereof

A nicosulfuron-methyl and crystal form technology is applied to the crystal form of nicosulfuron-methyl and the field of preparation thereof, which can solve the problems of not overcoming nicosulfuron-methyl and the like, achieve accurate calibration of product content, and ensure stability and accuracy. Effect

Inactive Publication Date: 2020-07-03
ZIBO NAB AGROCHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] But none of the crystals disclosed in the above-mentioned patent documents overcomes the problem that nicosulfuron is easy to absorb moisture

Method used

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  • Crystal form of nicosulfuron and preparation method thereof
  • Crystal form of nicosulfuron and preparation method thereof
  • Crystal form of nicosulfuron and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Take a clean 1000mL four-neck flask, put 800mL of acetonitrile into it, heat it in a water bath to 55°C while stirring (the boiling point of acetonitrile is 63°C), take 100g of high-content nicosulfuron original drug (all impurities are relatively low, content greater than or equal to 95%), put it into it, stir for 20min, use sand core funnel to suction filter while it is hot, and discard the filter residue;

[0032] (2) The filtrate is quickly placed in another clean 1000mL four-neck flask, and cooled naturally while stirring (if the room temperature is too low, use a water bath to cool naturally at 50°C) to room temperature, and pump it out with another clean sand core funnel. Filter, obtain the nicosulfuron pure product of 30g;

[0033] (3) Place the pure product in a constant temperature drying oven, and dry it for 5 hours at 60°C.

[0034] (4) Take another clean 1000mL four-neck flask, one side is connected with an oil-water separator, and the upper part is co...

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Abstract

The invention relates to nicosulfuron, in particular to a crystal form of nicosulfuron and a preparation method thereof. The crystal form of nicosulfuron is as shown in the specification. In an X-raypowder diffraction pattern of the crystal form, characteristic peaks appear when a reflection angle 2theta is equal to 12.4 + / - 0.2 degrees, 14.1 + / - 0.2 degrees, 15.4 + / - 0.2 degrees, 16.9 + / - 0.2 degrees, 18.3 + / - 0.2 degrees, 18.7 + / - 0.2 degrees, 21.8 + / - 0.2 degrees, 23.9 + / - 0.2 degrees, 24.7 + / - 0.2 degrees and 25.5 + / - 0.2 degrees. The preparation method comprises the following steps: carrying out recrystallizing by using acetonitrile, and carrying water by using toluene. The crystal form prepared by the method is not easy to absorb moisture; when the crystal form is used as a standardsample, the content of the standard sample used can be kept unchanged in half a year, so product content can be accurately calibrated, and the stability and accuracy of a nicosulfuron product detection system are guaranteed; and the preparation method is scientific, reasonable, simple and feasible.

Description

technical field [0001] The invention relates to nicosulfuron, in particular to a crystal form of nicosulfuron and a preparation method thereof. Background technique [0002] Nicosulfuron, whose chemical name is 2-(4,6-dimethoxypyrimidin-2-ylcarbamoylaminosulfonyl)-N,N-dimethylnicotinamide (English name Nicosulfuron), is a Japanese In the mid-1980s, Ishihara Sangyo Co., Ltd. discovered the sulfonylurea herbicide varieties for corn fields. Due to its high safety on corn, outstanding weeding effect, strong compatibility, and ultra-low mu dosage, etc. advantages and are popular. [0003] In the production enterprises of nicosulfuron technical and preparations, the storage and use of nicosulfuron standard samples has always been a difficult problem. Because there is an active hydrogen in the nicosulfuron molecule, it is easier to absorb moisture in the air, and the higher the content, the faster the moisture absorption speed. Often the purchased primary standard sample is calib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
CPCC07B2200/13C07D401/12
Inventor 邵长禄黄华李玉凤耿殿荣胡艳丽许鹏
Owner ZIBO NAB AGROCHEM
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