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Compound catalyst and application thereof

A technology of composite catalyst and etherification reaction, which is applied in the direction of catalytic reaction, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc. It can solve the complex, harsh and unfavorable industrial production of the preparation process, etc. question

Active Publication Date: 2016-05-04
PAPANNA BEIJING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of the catalyst is to suspend silica gel in toluene, add 3-chloropropyltrimethoxysilane under heating and reflux, reflux, cool, filter, wash and dry, and then mix the obtained solid with 2-hydroxymethyl-1, 4-diazabicyclo[2.2.2]octane and sodium hydride are heated to reflux in tetrahydrofuran, cooled, filtered, washed, and dried to obtain a catalyst for the etherification reaction of azoxystrobin, which can be recovered The preparation process of the catalyst is quite complicated and harsh, and the raw material cost is very high, so this catalyst is not conducive to the application of industrial production

Method used

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  • Compound catalyst and application thereof
  • Compound catalyst and application thereof
  • Compound catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1: the preparation of composite catalyst AW1

[0054] This example provides a preparation method of composite catalyst AW, specifically: add cuprous chloride 10g (99%, 0.101mol) and N,N-dimethylformamide 30ml in a 100ml there-necked flask, and stir at room temperature Add 11.3g (98%, 0.101mol) of 1,4-diazabicyclo[2,2,2]octane in 30mL of N,N-dimethylformamide solution, continue to react for 1h after adding, filter, The solid was washed twice with 40 ml of N,N-dimethylformamide, and dried to obtain 19.2 g of a reddish-brown product, ie composite catalyst AW1, with a yield of 90%.

Embodiment 2

[0055] Embodiment 2: the preparation of composite catalyst AW2

[0056] Compared with Example 1, the difference is only: cuprous chloride is replaced by cuprous iodide 19.23g (99.5%, 0.101mol), and 1,4-diazabicyclo[2,2,2]octane The alkane was replaced by equimolar 1,4-diazabicyclo[2,2,2]octane hydrochloride to obtain 27.8 g of a light green solid, namely composite catalyst AW2, with a yield of 90%.

Embodiment 3

[0057] Embodiment 3: the preparation of composite catalyst AW3

[0058] Compared with Example 1, the difference is only in that cuprous chloride is replaced by manganese chloride of equimolar number (manganese chloride tetrahydrate can be selected for use), and 27.8g dark brown solid product is obtained, that is, composite catalyst AW3, yield 89%.

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Abstract

The invention relates to a novel compound catalyst which is formed by compounding a compound A or / and salt thereof and a metal compound W, wherein the compound A has a structure as shown in a general formula I in the specification, in the general formula I, R1, R3, R5 and R6 are respectively hydrogen, halogen, C1-C10 oxygen or oxygen-free aliphatic hydrocarbon group, aryl, or ester group; and R2 and R4 are respectively hydrogen, halogen, or C1-C10 oxygen or oxygen-free aliphatic hydrocarbon group or aryl. The compound catalyst can be used for efficiently catalyzing the synthesis reaction of asymmetric 4,6-diaryloxy pyrimidine derivative, is stable in performance, can be recycled by a simple method, is reduced in catalyst consumption, avoids environment pollution, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a novel composite catalyst and its application in synthesizing asymmetric 4,6-bisaryloxypyrimidine derivatives. Background technique [0002] Asymmetric 4,6-bisaryloxypyrimidine derivatives, especially azoxystrobin and fluoxastrobin, as a class of high-efficiency, broad-spectrum fungicides, are widely used in the prevention and treatment of various plant diseases. [0003] The prior art discloses a method for preparing azoxystrobin with a copper halide as a catalyst; the method is to use (E)-2-[2-(6-chloropyrimidin-4-yloxy]phenyl]- Methyl 3-methoxyacrylate, salicylonitrile and potassium carbonate use copper halide as a catalyst to undergo etherification reaction in polar solvents, especially N,N-dimethylformamide, and filter to remove salt after the reaction And wash with N,N-dimethylformamide, the filtrate and the washing liquid are combined and decompressed to distill off the solvent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D239/52C07D413/12B01J31/32B01J31/30
CPCB01J31/1835B01J31/30B01J31/32B01J2231/4288B01J2531/0241B01J2531/16B01J2531/72C07D239/52C07D413/12B01J31/22Y02P20/584
Inventor 侯伟刘彬龙赵亚军朱丹张蒨
Owner PAPANNA BEIJING TECH