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Preparation apparatus and method of kresoxim-methyl intermediate

A technology for preparing equipment and intermediates, which is applied in the field of preparation equipment for kresoxim-methyl intermediates, which can solve the problems of insufficient control of reaction temperature, dropping time and molar ratio, many types of solvents used, low conversion rate and content, etc. Achieve the effects of easy industrial production, simple operation, and low production cost

Active Publication Date: 2016-08-24
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Liu Dongwei and others introduced a five-step method for preparing kresoxstrobin in the article "Research on the Synthesis of Fenoxystrobin" ("Fine Chemical Intermediates", 2003, 33 (4), 10-11). Although the method is basically similar to this patent, But the yield is only 57.2%, and there are many kinds of solvents used, poor product quality and other shortcomings
Patent WO9520569.1995 (Ziegler H, Neff D, Stutz W.Preparation of 2-aryl-2-(methoxyimino) acetate esters viapalladium-catalyzed cross-coupling reaction of aryl boronic acid and 2- (methoxyimino) acetateesters.) proposed to use Pd( Ph 3 P) 4 The patent describes two methods for synthesizing boric acid compounds. The first method has cumbersome steps, low yield and long reaction time. The second method has a slightly higher yield, but requires- 70 o The low temperature of C restricts the value of industrial production
[0006] In the existing production process, in the process of preparing the intermediate 2-(2-methylphenoxy)-methylene benzoyl cyanide, the reaction temperature, dropping time and molar ratio are not well controlled, resulting in low conversion rate and content

Method used

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  • Preparation apparatus and method of kresoxim-methyl intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 (sodium methoxide:o-cresol:phthalide molar ratio=0.95:1.02:1).

[0038] Slightly heat the reaction kettle one 1 and heat up to 50 o C, take 82.23g of liquid o-cresol (98% by mass) and add it to Reactor 1, then add 133.90g of sodium methoxide (28% by mass) to Reactor 1, and control the temperature of Reactor 1 to 58 o C, heat preservation for 1.5h, after heat preservation, add 100g of phthalide (mass fraction: 98%) to the reaction kettle 1, stir evenly, open the gas phase valve, raise the temperature to remove the methanol in the sodium methoxide, and raise the temperature to 80 o C, 7h to 155 o C, observe that the material turns red, no methanol is evaporated, stop stirring, keep warm for 3h, add 300g of water, and control the temperature at 75 o C, start stirring, after 0.5h, transfer to Reactor 25, slowly dropwise add 97g of hydrochloric acid (mass fraction: 30%) into Reactor 25, check the pH value, confirm that the pH value is 2, add 500ml of toluene, and...

Embodiment 2

[0039] Example 2 (sodium methoxide: o-cresol: phthalide molar ratio = 1:1.02:1).

[0040] Slightly heat the reaction kettle one 1 and heat up to 50 o C. Take 82.23 g of liquid o-cresol (98% by mass) and add it to Reactor 1, then add 140.9 g of sodium methoxide (28% by mass) to Reactor 1, and control the temperature of Reactor 1 to 58 o C, heat preservation for 1.5h, after heat preservation, add 100g of phthalide (mass fraction: 98%) to the reaction kettle 1, stir evenly, open the gas phase valve, raise the temperature to remove the methanol in the sodium methoxide, and raise the temperature to 80 o C, 7h to 155 o C, observe that the material turns red, no methanol is evaporated, stop stirring, keep warm for 3h, add 300g of water, and control the temperature at 75 o C, start stirring, after 0.5h, transfer to Reactor 25, slowly dropwise add 97g of hydrochloric acid (mass fraction: 30%) into Reactor 25, check the pH value, confirm that the pH value is 2, add 500ml of toluene, a...

Embodiment 3

[0041] Example 3 (sodium methoxide: o-cresol: phthalide molar ratio = 0.95:1:1).

[0042] Slightly heat reactor one 1, heat up to 50°C, take 80.62 g of liquid o-cresol (98% by mass fraction) and add it to reactor one 1, then add sodium methoxide (28% by mass fraction) 133.9 g to reactor one 1 g, control reactor one 1 temperature 58 o C, heat preservation for 1.5h, after heat preservation, add 100g of phthalide (mass fraction: 98%) to the reaction kettle 1, stir evenly, open the gas phase valve, raise the temperature to remove the methanol in the sodium methoxide, and raise the temperature to 80 o C, 7h to 155 o C, observe that the material turns red, no methanol is evaporated, stop stirring, keep warm for 3h, add 300g of water, and control the temperature at 75 o C, start stirring, after 0.5h, transfer to Reactor 25, slowly dropwise add 97g of hydrochloric acid (mass fraction: 30%) into Reactor 25, check the pH value, confirm that the pH value is 2, add 500ml of toluene, and...

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Abstract

The invention belongs to the technical field of organic synthesis and particularly relates to a preparation apparatus and method of kresoxim-methyl intermediate. The apparatus comprises a reactor, a condenser, a centrifuge, a material tank and a mass flow meter which are connected with one another; the method comprises: using phthalide, o-cresol and sodium methylate as materials, preparing 2-(2-methylphenoxy)-methylene benzoic acid first, and then preparing 2-(2-methylphenoxy)-methylene benzoyl cyanide through chlorination and cyanidation. The apparatus is simple in structure and reasonable in design; all materials are domestic, a single common solvent is selected, and recycling of the solvent enables reduced wastewater, reduced environmental load and reduced production cost; by optimizing process conditions, reaction conversion rate is increased, product content and yield are also increased, and the apparatus and method are suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to the synthesis technology of the fungicide kresoxim-methyl, in particular to a preparation device and method of a kresoxim-methyl intermediate. Background technique [0002] Kresstrobin is also known as phenoxystrobin, chemical name: (E)-2-methoxyimino-[2-(o-methylphenoxymethyl)phenyl]methyl acetate, molecular formula: C 18 h 19 NO 4 , molecular weight: 313.35, structural formula: [0003] . [0004] Kresoxim-methyl is a new semi-systemic methoxyacrylate fungicide. Patent CN201010130764.4 introduces the advantages of kresoxim-methyl in detail, which has the characteristics of wide sterilization range, high activity, long duration of drug properties, low toxicity, low residue and environmental friendliness. Since the listing of Syngenta's azoxystrobin and BASF's kysstrobin in 1996, Strobilurins (methoxyacrylate) fungicides have been tested by the market for more than...

Claims

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Application Information

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IPC IPC(8): C07C255/40C07C253/14
CPCC07C51/09C07C51/60C07C253/14C07C65/24C07C255/40
Inventor 丁金成卢杰吕恩民杜利雄马玲玲
Owner SHANDONG UNIV OF TECH
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