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Method for synthesizing epoxiconazole by catalyzing air or oxygen epoxidation

A technology for synthesizing epoxiconazole and epoxidation, which is applied in the direction of organic chemistry, can solve the problems of increased post-processing difficulty, increased production cost, and poor selectivity of waste acid, and achieve high product yield, reduction of three wastes, and The effect of high conversion rate of raw materials

Active Publication Date: 2014-11-12
SHENYANG SINOCHEM AGROCHEMICALS R&D CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent U.S.5245042 uses maleic anhydride and hydrogen peroxide to form monoperoxymaleic acid in situ to epoxidize triazolene, and uses 10 times the molar amount of maleic anhydride of triazolene, which increases the production of a large amount of waste acid The difficulty of post-processing has also brought great pressure to the environment; due to the use of hydrogen peroxide with a mass concentration of 50%, there are huge safety hazards in production; this process method is not selective, and a large amount of reducing agent must be added later to increase In order to reduce the production cost, the maximum selectivity is only 72% without adding reducing agent, and the yield is less than 62%.
Air or low-pressure oxygen are easy-to-get oxidants, and the method for preparing epoxiconazole by catalytic air oxidation or oxygen oxidation of triazolene has not been reported

Method used

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  • Method for synthesizing epoxiconazole by catalyzing air or oxygen epoxidation
  • Method for synthesizing epoxiconazole by catalyzing air or oxygen epoxidation
  • Method for synthesizing epoxiconazole by catalyzing air or oxygen epoxidation

Examples

Experimental program
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Effect test

Embodiment 1

[0025] In a glass reactor, dissolve 0.03g (0.05mmol) tris(dibenzoylmethane)iron, 0.78g (2.5mmol) triazolene, 1.08g (14.9mmol) isobutyraldehyde in 20mL 1,2-dichloroethyl In alkanes, the temperature was raised to 50° C. with stirring, and air at one atmosphere was maintained, and kept stirring at this temperature for 18 hours. Heating was stopped, the material was naturally cooled to room temperature, and sampling analysis showed that the conversion of triazole was 87.0%, the selectivity of epoxiconazole was 78.1%, and the yield of epoxiconazole was 67.9%.

Embodiment 2

[0027] Use 0.15g (0.25mmol) tris(dibenzoylmethane)iron instead, other conditions are the same as in Example 1, stir at room temperature for 24 hours, heat up to 50°C and react at this temperature for 8 hours, stop heating, and let the material cool naturally to room temperature. Sampling analysis showed that the conversion rate of triazolene was 76.3%, the selectivity of epoxiconazole was 78.0%, and the yield of epoxiconazole was 59.5%.

Embodiment 3

[0029] In a glass reactor, dissolve 0.14g (0.28mmol) bis(dibenzoylmethane) cobalt, 0.78g (2.5mmol) triazolene, 1.08g (14.9mmol) isobutyraldehyde in 10mL 1,2-dichloroethyl In alkanes, keep one atmospheric pressure of air, stir at room temperature for 19 hours, be warmed up to 50 ° C and react at this temperature for 8 hours, stop heating, and the material is naturally cooled to room temperature. Sampling analysis showed that the conversion rate of triazolene was 71.0%, the selectivity of epoxiconazole was 77.0%, and the yield of epoxiconazole was 54.7%.

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Abstract

The invention belongs to the field of organic synthesis, and concretely relates to a method for synthesizing epoxiconazole by catalyzing air or oxygen epoxidation. Triazo alkene is epoxidized under the catalysis of a metal cobalt and iron organic catalyst with air or oxygen as an oxidant and aldehyde as an oxygen acceptor. A reaction formula is shown in the specification. The catalytic epoxidation reaction has the advantages of simple operation, high raw material conversion rate and high yield, and is suitable for the large scale preparation of epoxiconazole. In the formula, Cat represents the metal cobalt and iron organic catalyst.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for synthesizing epoxiconazole by catalytic air or oxygen epoxidation. technical background [0002] Epoxiconazole is a broad-spectrum triazole fungicide with high efficiency, low toxicity and low residue, which was developed by BASF in 1985. It has been reported in the literature that there are six routes for the synthesis of epoxiconazole. In industrial production, hydrogen peroxide and maleic anhydride are used to generate peracid in situ and react with triazolene to synthesize epoxiconazole. Patent U.S.5245042 uses maleic anhydride and hydrogen peroxide to form monoperoxymaleic acid in situ to epoxidize triazolene, and uses 10 times the molar amount of maleic anhydride of triazolene, which increases the production of a large amount of waste acid The difficulty of post-processing has also brought great pressure to the environment; due to the use of hydrogen peroxide ...

Claims

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Application Information

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IPC IPC(8): C07D405/06
CPCC07D405/06
Inventor 姜鹏孟志
Owner SHENYANG SINOCHEM AGROCHEMICALS R&D CO LTD
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