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Azabicyclic complex catalyst, and preparation method and application thereof

A technology of azabicyclic and complexes, which is applied in the field of azabicyclic tertiary amine complex catalysts and its preparation, and can solve the problems of high catalyst price, low yield, and environmental pollution

Active Publication Date: 2019-09-27
内蒙古灵圣作物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] Above prior art adopts azabicyclic tertiary amine compound as the catalyst of etherification reaction, conversion rate is about 92-95%, there is the problem of low yield, the crude product that obtains also needs to carry out recrystallization, just can obtain relatively High-purity products. In addition, azabicyclic tertiary amines have the characteristics of easy sublimation, forming organic volatiles and polluting the environment. In the later stage of the etherification reaction process, catalysts need to be supplemented. The price of catalysts is high, and the synthesis reaction process is uneconomical.

Method used

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  • Azabicyclic complex catalyst, and preparation method and application thereof
  • Azabicyclic complex catalyst, and preparation method and application thereof
  • Azabicyclic complex catalyst, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1-6

[0076] The preparation of embodiment 1-6 azabicyclic tertiary amine complex catalyst

[0077] Embodiment 1-6 adopts the method of the present application to prepare the azabicyclic tertiary amine complex catalyst of the present invention, and the yield of the azabicyclic tertiary amine complex is more than 85%, and embodiment 1 and 3 have used The previous batch of mother liquor was used as the reaction solvent, and the yield reached more than 95%.

Embodiment 1

[0078] Embodiment 1: Adopt cuprous bromide and last batch of mother liquor to prepare formula Ⅰ-2 complex

[0079] (1) Pretreatment of cuprous bromide

[0080] The cuprous bromide purchased by industrial production or reagent companies contains a small amount of copper bromide, and the color is light green. In order to ensure the catalytic effect, pretreatment is required.

[0081] Add 450g of 3% dilute HBr into the four-neck flask, add 0.5gNa 2 SO 3 , remove the bromine or oxygen in the oxidation state in dilute HBr, and at the same time reduce the divalent copper ions to cuprous ions, quickly add 1000g of reagent-grade CuBr, replace it with high-purity nitrogen three times, stir at room temperature for about 2 hours, Since CuBr is insoluble in dilute HBr, and CuBr 2 Soluble in dilute HBr, to achieve the purpose of separation and purification, filter under nitrogen protection, rinse twice with absolute ethanol to remove moisture, and vacuum dry at 50-60°C for 2 hours to ...

Embodiment 2

[0086] Embodiment 2: Adopt cuprous bromide to prepare formula Ⅰ-2 complex

[0087] (1) the pretreatment method of cuprous bromide is the same as embodiment 1

[0088] (2) Preparation of formula Ⅰ-2

[0089] Measure 400mL of anhydrous acetonitrile, start stirring, then add 287.48g of cuprous bromide (99.7%) powder, under nitrogen protection, heat to 45-50°C to dissolve, and it becomes a light gray solution, which is set aside.

[0090] In the four-necked bottle, add 126.20g of 2-methyltriethylenediamine, add 200mL of acetonitrile, dissolve at room temperature, fill with nitrogen protection, and use a constant pressure feeding funnel to drop the cuprous bromide solution prepared above into , the temperature is 20-30°C, about 20 minutes after the addition, the light brown ligand compound is continuously precipitated, after the addition is completed, stir at room temperature for 1 hour, then cool down to -10°C, crystallize, and filter with nitrogen protection to avoid inhalatio...

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Abstract

The invention relates to an azabicyclo tertiary amine complex catalyst and a preparation method thereof. The azabicyclo tertiary amine complex catalyst can be used for synthesizing methyl 2-[2-[6-chloropyrimidin-4-yloxy]phenyl]-3,3-dimethoxypropanoate (III) and methyl (E)-2-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]methoxyacrylate (V). The catalyst can significantly increase the yield of an etherification reaction, and can be used to obtain a product having a purity of above 99.4% and a white color.

Description

technical field [0001] The invention relates to an azabicyclic tertiary amine complex catalyst and a preparation method thereof. The azabicyclic tertiary amine complex catalyst is applicable to the synthesis of (2-[2-[6-chloropyrimidin-4-yl Oxy]phenyl]-3,3-dimethoxypropionic acid methyl ester (Ⅲ) and (E)-2-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy Base] phenyl] -3-methoxymethyl acrylate (Ⅴ) special catalyst. Background technique [0002] (E)-2-[2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl]-3-methoxymethyl acrylate is an efficient and broad-spectrum agricultural fungicide It has multiple functions such as systemic conduction, prevention, protection and treatment, and has good control effects on powdery mildew, rust, glume blight, downy mildew and rice blast of plants. At present, the industrial synthesis methods with economic value are all using (E)-2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxymethyl acrylate and o-hydroxybenzonitrile Reaction preparation. The specific...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07F1/08C07D239/34C07D239/52
CPCB01J31/183C07F1/08C07D239/34C07D239/52B01J2531/16B01J2231/482B01J2231/40
Inventor 时叶强曹彤彤
Owner 内蒙古灵圣作物科技有限公司
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