81777-89-1Relevant articles and documents
Preparation method of 2-(2-chlorphenyl)methyl-4, 4-dimethyl-3-isoxazolone
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Paragraph 0013-0048, (2021/11/10)
The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of 2-(2-chlorphenyl)methyl-4, 4-dimethyl-3-isoxazolone. The method comprises the following steps: by taking 4, 4-dimethyl-3-isoxazolone and o-chlorobenzyl chloride as raw materials, in the presence of an acid-binding agent, controlling the pH value of a reaction system to be 8.5-9.5, reacting, and after the reaction is finished, performing post-treatment to finally prepare the 2-(2-chlorphenyl)methyl-4, 4-dimethyl-3-isoxazolone. The method has the advantages of high conversion rate and yield, few byproducts and simple post-treatment of the product, conforms to the concept of green circular economy, and solves the technical problems of low conversion rate, more impurities in the chloropivaloyl chloride oximation reaction, low product quality and the like in the original o-chlorobenzaldehyde oximation method.
Preparation method of clomazone
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Paragraph 0003-0004, (2021/06/26)
The invention relates to a preparation method of clomazone. The method comprises: by taking hydroxylamine hydrochloride as a raw material, dropwise adding chloro pivaloyl chloride under the action of a self-made ether catalyst to obtain an intermediate 3-chloro-N-hydroxyl-2, 2-dimethyl propionamide with high yield, then cyclizing to prepare 4, 4-dimethyl-3-isoxazolone, and carrying out benzylation under pioneered caustic soda flake catalysis without separation to directly prepare 2-(2-chlorphenyl) methyl-4, 4-dimethyl-3-isoxazolone. Compared with existing literature methods, the method of the invention has the advantages that the self-made ether catalyst is innovatively used, so that the yield in the first step is remarkably improved, and the content and optical purity of the product are high; in the final benzylation reaction, caustic soda flakes are used to improve the yield, and water is used as a solvent in the whole reaction process, so that the cost is low, the recovery and post-treatment are simple, the reaction is mild, and the intermediate control is simple; and the preparation method provided by the invention has the advantages of easily available reaction raw materials, mild reaction, high yield, simple separation and purification, low cost and environment-friendly preparation process.
Preparation method of high-content clomazone
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Paragraph 0005; 0021-0032, (2021/07/21)
The invention discloses a preparation method of high-content clomazone, which comprises the following steps: putting an aqueous solution of 4,4-dimethyl-3-isoxazolone sodium salt, sodium carbonate and sodium iodide into a reaction kettle, pumping o-chlorochlorobenzene, and stirring and heating the reactants; keeping the temperature and reacting for 1.5-3 hours; performing sampling and central control, and then washing, layering and desolventizing the reaction product to obtain a crude clomazone product. A small amount of sodium chloride is added in the synthesis process of the clomazone, so that the reaction speed is greatly increased, the reaction time is shortened from 10 hours to 2 hours, the main content can reach 85% or above, and by-products are reduced to 3% or below.
Method for producing carbendazim by electrodialysis method and production device thereof (by machine translation)
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, (2020/04/17)
The apparatus, disclosed by the invention comprises a bipolar membrane electrodialysis reactor and a reaction kettle, bipolar membrane electrodialysis reactor which are further, communicated with sulfuric acid tank and hydrochloric acid tank N - (2 - to generate) - chlorine (N-benzyl, N - (2 - hydroxylamine) - chlorine-benzyl, hydroxyl - 2222, 2-dimethyl-propionamide, chloride - N N N N N-Bethanesulfonyl chloride, for generating and killing methyl 3 - hydroxyl - 2222,2-dimethyl-propionamide under alkaline condition is produced) - N - chlorine - N N N N N-propionamide under alkaline condition.3 - The production device disclosed by the, invention has the advantages of high, production efficiency) - N - yield, high, product quality; and the like in the electrolysis process, discloses a bipolar membrane electrodialysis reaction method, and a bipolar membrane electrodialysis reaction, still, liquid, produced by using a bipolar membrane electrodialysis, method and a double-polar membrane electrodialysis reactor. (by machine translation)
Low-temperature synthesis process of clomazone
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Paragraph 0025; 0028; 0031; 0034; 0037; 0040, (2019/09/05)
The invention discloses a low-temperature synthesis process of clomazone. The low-temperature synthesis process of the clomazone comprises condensation reaction, cyclization reaction, synthesis reaction and configuration conversion. The low-temperature synthesis process of the clomazone disclosed in the invention starts from analyzing side reaction products, determines the chemical composition ofimpurities, and reduces the amount of the impurities by optimizing process parameters, finding high-efficiency catalysts and controlling side reactions; then, through chemical treatment on the produced isomers, part of the isomers are converted into the product, and part of irreversible by-products are converted into high-boiling-point polymer compounds through reaction, so that the clomazone product is easy to separate; finally, the clomazone product is purified through physical methods to obtain the clomazone with a purity greater than 97%.
A method for preparing clomazone through bipolar membrane electrodialysis
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Page/Page column 5; 6; 7, (2018/12/01)
A method for preparing clomazone through bipolar membrane electrodialysis is disclosed. Hydroxylamine hydrochloride and chloropivaloyl chloride are reacted through a bipolar membrane electrodialysis device; then a sodium chloride solution is added to continue the reaction through the bipolar membrane electrodialysis device; and finally 2-chlorobenzyl chloride in an equal mole is added and a phasetransfer catalyst is added for a reaction to obtain a crude clomazone product. The method has advantages of high production efficiency, energy consumption reducing, clean production, and the like, andhas innovative directing meanings for other pesticide production enterprises.
Preparation method of clomazone
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Paragraph 0018; 0021; 0024; 0027, (2017/08/29)
The invention relates to a preparation method of clomazone, wherein an intermediate, 4,4-dimethylisoxazole-3-one, is synthesized by dropwise adding chloro-pivaloyl chloride to a raw material, hydroxylamine hydrochloride, under the effects of a self-made ether catalyst; and then the intermediate is condensed with o-chlorobenzyl chloride under the effects of a caustic soda flake catalyst to synthesize a raw drug of the clomazone. The preparation method uses easy-to-obtained raw materials and mild reactions, is high in yield and is simple in separation and purification, has low cost, is environment-friendly, and has great industrial application prospect.
PROCESS FOR PREPARING CLOMAZONE, NOVEL FORM AND USE OF THE SAME
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Page/Page column 16; 17, (2015/01/16)
A process for preparing clomazone is provided,the process comprising reacting 4,4-dimethyl-3-isoxazolidinone with 2-chlorobenzyl chloride in an aqueous medium in the presence of a base, in particular an alkali metal hydroxide. A method for preparing clomazone is also disclosed, the method comprising (a) crystallizing clomazone from solution in an organic solvent; and (b) isolating the resulting crystals. N-benzene is a particularly suitable solvent. Further, there is provided Form I crystalline 2-[(2-chlorophenyl)methyl]-4,4-dimethyl-3-isoxazolidinone (clomazone), wherein the polymorph Form I is characterized by at least one of the following properties : (i) an X-ray powder diffraction pattern having characteristic peaks expressed in degrees 2θ(+/-0.20° θ) at one or more of the following positions : about 10.63, 16.07, 18.08, 19.11, 19.34, 21.20, 24.78 and 28.80; and (ii) an infrared (IR) spectrum having a characteristic peak : at about 2967 and 2870 cm-1.
Variable Release Water Dispersible Granule Composition
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Page/Page column, (2014/09/30)
A water dispersible granule composition comprising microcapsules comprising at least one agrochemical active ingredient encapsulated within a urea formaldehyde polymeric shell wall, at least one inert filler and at least one agrochemical excipients.
Herbicidal mixtures having a synergistic effect
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, (2008/06/13)
PCT No. PCT/EP96/03996 Sec. 371 Date Feb. 17, 1998 Sec. 102(e) Date Feb. 17, 1998 PCT Filed Sep. 12, 1996 PCT Pub. No. WO97/10714 PCT Pub. Date Mar. 27, 1997A composition comprising at least one sulfonylurea of the formula I wherein R1 is substituted alkyl; halogen; a group ER6 (E=O, S or NR7); COOR8; NO2; S(O)oR9; SO2NR10R11; or CONR10R11; R2 is hydrogen, alkyl, alkenyl, alkynyl, halogen, alkoxy, haloalkoxy, haloalkyl, alkylsulfonyl, nitro, cyano or alkylthio; R3 is F, CF3, CF2Cl, CF2H, OCF3, OCF2Cl, or, if R1 is CO2CH3 and R2 is simultaneously fluorine, R3 is Cl, or, if R1 is CH2CF3 or CF2CF3, R3 is methyl, or, if R4 is OCF3 or OCF2Cl, R3 is OCF2H or OCF2Br; R4 is alkoxy, alkyl, alkylthio, alkylamino, dialkylamino, halogen, haloalkyl or haloalkoxy; and R5 is hydrogen, alkoxy or alkyl; or an enviromentally compatible salt of I, and an aryloxyalkanoic acid selected from the group consisting of 2,4-D, 2,4-DB, clomeprop, dichlorprop, dichlorprop-P, dichlorprop-P (2,4-DP-P), fenoprop (2,4,5-TP), fluoroxypyr, MCPA, MCPB, mecoprop, mecoprop-P, napropamide, napropanilide, triclopyr, and an enviromentally compatible salt thereof exhibits a synergistic herbicidal effect.