Refined glufosinate acid aquo-complex crystals and preparation method thereof

A technology of hydrate and ammonium glufosin, which is applied in the field of pesticides, can solve the problems of differences in bioavailability, achieve good fluidity, improve the quality of drug production, and make the preparation method simple and easy to operate

Inactive Publication Date: 2019-02-22
SHANDONG ACADEMY OF PESTICIDE SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Different crystal forms of the same drug may have significantly different bioavailability

Method used

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  • Refined glufosinate acid aquo-complex crystals and preparation method thereof
  • Refined glufosinate acid aquo-complex crystals and preparation method thereof
  • Refined glufosinate acid aquo-complex crystals and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] First, add refined glufosinate-ammonium hydrochloride (1mol) into 200ml of water and 200ml of methanol, heat up to 60°C to dissolve, cool down to 30°C, and feed 18.7g of ammonia gas; then, stir at room temperature for 20 minutes, cool down Stir at -10°C for 3 hours to crystallize, filter the precipitated crystals, wash with methanol and dry to obtain 179.1 g of refined glufosinate-ammonium monohydrate crystals with a yield of 90% and a purity of 98%.

Embodiment 2

[0040] First, add refined glufosinate-ammonium hydrochloride (1mol) into 100ml of water and 300ml of methanol, heat up to 60°C to dissolve, cool down to 30°C, and feed 18.7g of ammonia gas; then, stir at room temperature for 20 minutes, cool down Stir at -5°C for 3 hours to crystallize, filter the precipitated crystals, wash with methanol and dry to obtain 185.1 g of refined glufosinate-ammonium monohydrate crystals with a yield of 93% and a purity of 97.9%.

Embodiment 3

[0042] First, add refined glufosinate-ammonium hydrochloride (0.1mol) into 20ml of water, heat up to 60°C to dissolve it, cool down to 30°C, and add 7.3g of concentrated ammonia water with a concentration of 28% dropwise; then, stir at room temperature for 15 minutes, Cool down to -10°C, stir for 5 hours to crystallize, filter the precipitated crystals, wash with methanol and dry to obtain 16 g of refined glufosinate-ammonium monohydrate crystals with a yield of 80.4% and a purity of 97.8%.

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Abstract

The invention belongs to the field of pesticides and discloses refined glufosinate acid aquo-complex crystals and a preparation method thereof. The refined glufosinate acid aquo-complex crystals are refined glufosinate acid-aquo-complex crystals. An X-ray powder diffraction spectrogram represented by diffraction angles: 2theta+/-0.2 degrees of the quo-complex crystals shows characteristic diffraction peaks (shown as a figure 1) at 2theta: 14.67 degrees, 17.17 degrees, 20.83 degrees, 22.23 degrees, 22.43 degrees, 23.12 degrees, 25.99 degrees, 27.66 degrees, 30.68 degrees, 34.69 degrees and 41.34 degrees. The characteristic diffraction peaks are obviously different from those in the prior art. The refined glufosinate acid-aquo-complex crystals have good performance and are quite suitable foractual applications. The invention also discloses a preparation method for the refined glufosinate acid-aquo-complex crystals. The preparation method is simple and mild and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of pesticides, and in particular relates to a crystal of refined glufosinate-ammonium acid hydrate and a preparation method thereof. Background technique [0002] Glufosinate-ammonium is a high-efficiency, low-toxicity, broad-spectrum non-selective herbicide widely used to control annual and perennial dicotyledonous and gramineous weeds. The chemical name of refined glufosinate-ammonium: 4-[hydroxy (methyl) phosphono]-L-homoalanine; CAS number: [35597-44-5]; its molecular formula is: C 5 h 12 NO 4 P, molecular weight: 181.1; structural formula: [0003] [0004] Those skilled in the art know that the polymorphic form of a drug has become an essential and important part in the process of drug research and drug production quality control and testing. Different crystal forms of the same drug may have significantly different bioavailability. For the same drug, some crystal forms may have higher biological activity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07B2200/13C07F9/301
Inventor 董文凯柴洪伟解银萍李磊韩金涛刘军王滢秀徐玉梅左伯军李旭坤
Owner SHANDONG ACADEMY OF PESTICIDE SCI
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