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Method for producing glufosinate P free acid

A manufacturing method and glufosinate-ammonium technology are applied in the manufacturing field of glufosinate-ammonium P free acid, which can solve the problems of high hygroscopicity and complicated post-processing procedures, and achieve the effect of low hygroscopicity

Active Publication Date: 2014-05-28
MMAG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since there is a problem that the post-processing process is complicated, and the obtained powder is amorphous, it has very high hygroscopicity and has industrial problems.

Method used

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  • Method for producing glufosinate P free acid
  • Method for producing glufosinate P free acid
  • Method for producing glufosinate P free acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Embodiment 1: the manufacture of glufosinate-ammonium P free acid

[0080] 50 mmol of glufosinate-ammonium P hydrochloride was dissolved in 10 mL of water and 90 mL of methanol, and 25 mL of methanol in which 1 N of sodium hydroxide was dissolved was added thereto. The seed crystal obtained in Reference Example 2 was added, stirred at room temperature for 15 minutes, then cooled with ice and stirred for 3 hours and 30 minutes, and the precipitated crystals were collected by filtration. This was vacuum-dried to obtain 9.35 g of the title compound (recovery rate: 95.9%, purity: 91.7%).

Embodiment 2

[0081] Embodiment 2: the manufacture of glufosinate-ammonium P free acid

[0082] 50 mmol of glufosinate-ammonium P hydrochloride was dissolved in 17 mL of water, and 4.17 g of water in which 1 N of sodium hydroxide was dissolved was added thereto. 60 mL of methanol was added thereto, and the seed crystal obtained in Reference Example 2 was added, stirred at room temperature for 15 minutes, then cooled with ice and stirred for 3 hours and 30 minutes, and the precipitated crystals were filtered out. This was vacuum-dried to obtain 9.09 g of the title compound (recovery rate: 92.4%, purity: 92.0%).

Embodiment 3

[0083] Embodiment 3: the manufacture of glufosinate-ammonium P free acid

[0084] 50 mmol of glufosinate-ammonium P hydrochloride was dissolved in 20 mL of water and 180 mL of methanol, and 1 N of sodium hydroxide was added thereto. The seed crystal obtained in Reference Example 2 was added, stirred at room temperature for 15 minutes, then cooled with ice and stirred for 3 hours and 30 minutes, and the precipitated crystals were collected by filtration. This was vacuum-dried to obtain 9.09 g of the title compound (recovery rate: 91.3%, purity: 98.8%).

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Abstract

Provided is a method for producing high-purity crystals of a glufosinate P free acid from glufosinate P hydrochloride. The provided method comprises a step for dissolution of glufosinate P hydrochloride in a solvent, which is a mixed solvent of water and an alcohol selected from methanol, ethanol, propyl alcohol, or isopropyl alcohol having a water:alcohol ratio of 1:3 to 1:100; adding a base for neutralization; and crystallizing the glufosinate P free acid.

Description

technical field [0001] [Remarks about related applications] [0002] This invention claims priority based on Japanese Patent Application No. 2011-217141 (filed on September 30, 2011), and the entire description content of this application is incorporated in this specification by reference. [0003] The present invention relates to a novel process for the manufacture of glufosinate-ammonium P free acid useful as a herbicide. Background technique [0004] Glufosinate-ammonium P (L-2-amino-4-(hydroxymethylphosphinyl)-butyric acid) is glufosinate-ammonium (DL-2-amino-4-(hydroxymethylphosphinyl)-butyric acid) It is widely used as an active ingredient of herbicides. As a general method concerning the manufacturing method of glufosinate-ammonium and glufosinate-ammonium P, there exist the following methods, for example. [0005] (1) In the presence of glutamic acid or a salt thereof and aspartic acid or a salt thereof as amino donors, 4-(hydroxymethylphosphinyl)-2 is converted b...

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 中西希安藤孝箕轮宣人三富正明
Owner MMAG CO LTD
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