82785-28-2Relevant academic research and scientific papers
CRYSTALLINE FORM OF L-GLUFOSINATE AMMONIUM SALT AND PROCESS FOR PRODUCTION THEREOF
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Page/Page column 26-29, (2022/02/09)
The present disclosure relates to a novel crystalline form of L-glufosinate ammonium salt and a process for preparation thereof. The present disclosure also provides compositions comprising said form and a method for the control of undesired plant growth using said compositions.
Highly Stable Zr(IV)-Based Metal-Organic Frameworks for Chiral Separation in Reversed-Phase Liquid Chromatography
Jiang, Hong,Yang, Kuiwei,Zhao, Xiangxiang,Zhang, Wenqiang,Liu, Yan,Jiang, Jianwen,Cui, Yong
supporting information, p. 390 - 398 (2021/01/13)
Separation of racemic mixtures is of great importance and interest in chemistry and pharmacology. Porous materials including metal-organic frameworks (MOFs) have been widely explored as chiral stationary phases (CSPs) in chiral resolution. However, it remains a challenge to develop new CSPs for reversed-phase high-performance liquid chromatography (RP-HPLC), which is the most popular chromatographic mode and accounts for over 90% of all separations. Here we demonstrated for the first time that highly stable Zr-based MOFs can be efficient CSPs for RP-HPLC. By elaborately designing and synthesizing three tetracarboxylate ligands of enantiopure 1,1′-biphenyl-20-crown-6, we prepared three chiral porous Zr(IV)-MOFs with the framework formula [Zr6O4(OH)8(H2O)4(L)2]. They share the same flu topological structure but channels of different sizes and display excellent tolerance to water, acid, and base. Chiral crown ether moieties are periodically aligned within the framework channels, allowing for stereoselective recognition of guest molecules via supramolecular interactions. Under acidic aqueous eluent conditions, the Zr-MOF-packed HPLC columns provide high resolution, selectivity, and durability for the separation of a variety of model racemates, including unprotected and protected amino acids and N-containing drugs, which are comparable to or even superior to several commercial chiral columns for HPLC separation. DFT calculations suggest that the Zr-MOF provides a confined microenvironment for chiral crown ethers that dictates the separation selectivity.
L-glufosinate ammonium salt crystal form, preparation method and application thereof
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Paragraph 0033-0044; 0056-0057, (2022/01/08)
The invention relates to the technical field of pesticides, and particularly discloses an L-glufosinate ammonium salt crystal form, a preparation method and application thereof. The crystal form of the L-glufosinate ammonium salt has characteristic diffraction peaks at the positions of 2theta+/-0.2 degrees which are equal to 9.10 degrees, 10.05 degrees, 16.77 degrees, 17.67 degrees, 18.30 degrees, 18.83 degrees, 23.47 degrees, 24.10 degrees, 25.61 degrees, 28.55 degrees, 29.01 degrees and 33.40 degrees. In the novel crystal form of L-glufosinate ammonium, the molar ratio of glufosinate ammonium to ammonium ions is close to 1: 1, the ammonium ion content is high, the crystal form stability is good, the ammonia content is not obviously reduced after long-time storage, the crystal form structure is not changed, the hygroscopicity is low, development, preparation and storage of weeding drug products are facilitated, and the novel crystal form has high application and popularization value.
Weeding composition compounded by fine glufosinate-ammonium and diuron and preparation method and application thereof
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Paragraph 0030, (2021/08/07)
The invention provides a weeding composition compounded by fine glufosinate-ammonium and diuron. The weeding composition is characterized by comprising fine glufosinate-ammonium, diuron and other auxiliary agents, and the content of the fine glufosinate-ammonium is 1-60 parts by mass, the content of the diuron is 1-60 parts by mass, and the content of the auxiliary agents is 20-70 parts by mass. By reasonably proportioning the proportions of the fine glufosinate-ammonium and the diuron in the herbicide, the pesticide effect of the herbicide is enhanced, the control effect on weeds in uncultivated areas is superior to the activity of the singly applied components, meanwhile, the control spectrum of the weeds is expanded, the weeding effect is improved, the weeding composition has a prominent comprehensive control effect on gramineous weeds, cyperaceae weeds and broadleaf weeds, and has the advantages of fast effectiveness, long lasting period, delayed herbicide resistance, thorough weeding, low residue, low toxicity, safety, environmental protection and the like.
Method for preparing phosphorus-containing a-aminonitriles
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Paragraph 0148; 0158, (2021/06/22)
The present invention relates primarily to processes conducted in a continuously operated reactor for preparing particular phosphorus-containing α-aminonitriles of the formulae (Ia) and (Ib) defined hereinafter from corresponding phosphorus-containing cyanohydrin esters and to the use thereof for preparation of glufosinate or of glufosinate salts. The present invention further relates to a process for producing glufosinate/glufosinate salts.
Synthesis method of glufosinate-ammonium
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Paragraph 0038-0082, (2021/07/01)
The invention relates to the field of pesticides, in particular to a synthesis method of glufosinate-ammonium. The synthesis method of glufosinate-ammonium comprises the following steps: reacting a mixed aqueous solution of a hydantoin derivative, volatile alkali and a catalyst under 1.0-2.5 MPa, and after the reaction is finished, carrying out post-treatment to obtain glufosinate-ammonium, wherein the catalyst is a guanidine compound. The synthesis method of glufosinate-ammonium provided by the invention jumps out of the thought of separating glufosinate-ammonium from inorganic salt in the prior art, creatively adopts the mutual cooperation of volatile alkali and the catalyst (guanidine compound), and hydrolyzes the hydantoin derivative under the specific pressure of 1.0-2.5 MPa, so that the hydantoin compound is thoroughly hydrolyzed, the yield of glufosinate-ammonium is improved, meanwhile, the reaction time is shortened, acid-base neutralization is not needed after the reaction is finished, inorganic salt is not generated, generation of the inorganic salt in the glufosinate-ammonium preparation process is fundamentally eradicated, three wastes are not generated, the yield of glufosinate-ammonium is high, and industrial popularization is easy.
Preparation method of L-glufosinate-ammonium
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Paragraph 0017-0020, (2020/05/08)
The invention discloses a preparation method of L-glufosinate-ammonium, and the method comprises the following steps: by using DL-glufosinate-ammonium as a starting raw material, complexing the DL-glufosinate-ammonium with a chiral auxiliary group and metal ions under the action of an inorganic alkali to form a coordination compound, and inversing the configuration of D-glufosinate-ammonium in theprocess to generate the L-glufosinate-ammonium. And by hydrolyzing the coordination compound, the L-glufosinate-ammonium is obtained, and meanwhile the chiral auxiliary group and the metal salt are recovered. The method is simple in process route, high in yield, low in cost and suitable for industrial production of the L-glufosinate-ammonium.
Process for preparing phosphorus-containing alpha-aminonitriles
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Paragraph 0096-0099, (2020/06/08)
The present invention relates primarily to processes for preparing particular phosphorus-containing α-aminonitriles of the formulae (Ia) and (Ib) defined hereinafter from corresponding phosphorus-containing cyanohydrin esters and to the use thereof for preparation of glufosinate or of glufosinate salts. The present invention further relates to a process for preparing glufosinate or glufosinate salts.
Preparation method of glufosinate-ammonium
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Paragraph 0021; 0037-0043, (2020/05/01)
The invention discloses a preparation method of glufosinate-ammonium. According to the method, methyl phosphine dichloride is used as a raw material, and reacts with acrolein under the action of acetic anhydride to obtain an unsaturated phosphine-containing heterocyclic ring represented by a formula I; a hydrolysis reaction is performed to obtain a phosphine aldehyde intermediate represented by aformula II; the phosphine aldehyde intermediate is subjected to a strecker reaction to obtain an amino nitrile intermediate; and the amino nitrile intermediate is sequentially subjected to a hydrolysis reaction and a salifying reaction to obtain glufosinate-ammonium. According to the invention, the preparation method is short in technological process, and particularly can directly obtain the phosphine aldehyde intermediate without diethyl methylphosphite, so that the production cost of glufosinate-ammonium can be greatly reduced, and the further commercial popularization of glufosinate-ammonium is facilitated; and the method has good environmental friendliness, avoids the wastewater generated by the Grignard reaction in the traditional method, and also has no great potential safety hazard.
Method for synthesizing glufosinate ammonium salt
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Paragraph 0103; 0115-0116; 0123; 0135-0137; 0149-0150, (2019/11/13)
The invention discloses a method for synthesizing a glufosinate ammonium salt. The method comprises the following steps that (1) methyldiethoxyphosphine and n-butanol are used as raw materials to produce an intermediate I by hydrolysis and transesterification; (2) the intermediate I is subjected to a free radical addition reaction with acrolein cyanohydrin acetate to form an intermediate II; (3) the intermediate II is subjected to an aminolysis reaction with ammonia gas to form a mixture of an intermediate III and an intermediate IV; (4) the intermediate III and the intermediate IV are subjected to acid hydrolysis with hydrochloric acid to form an intermediate V; and (5) the intermediate V is neutralized, purified and crystallized to obtain the glufosinate ammonium salt. The method does not need to use toxic raw materials, avoids the large-scale use of ammonia water and ammonium chloride, not only greatly reduces the safety hazard, but also reduces the quantity of by-products and the amount of waste water generated, and the environmental protection risk is greatly reduced; and the purification process is simple, the product content and the yield coefficient are obviously increased,and the method is suitable for industrial scale production.
