Method for synthesizing 2(3H)-benzofuranone by utilizing microwave

A technology for benzofuranone and microwave synthesis, which is applied in the direction of organic chemistry, can solve the problems of yellowish color of benzofuranone, low yield of recrystallization crystallization, and increased environmental cost, so as to reduce polymerization, reduce dehydration temperature, The effect of easy operation
CN102887879AInactive Publication Date: 2013-01-23JIANGSU SWORD AGROCHEM
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
JIANGSU SWORD AGROCHEM
Publication Date
2013-01-23
Estimated Expiration
Not applicable · inactive patent
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Abstract

The invention discloses a method for synthesizing 2(3H)-benzofuranone by utilizing microwave, which comprises the following steps: after making o-chloro or o-bromo, o-iodophenylacetic acid react at a high temperature or a high temperature and a high pressure, acidifying the material, extracting the raw material without any solvent, and then directly dehydrating the material under a negative pressure, directly transferring the material into a microwave reactor with a stirrer, setting power; after monitoring the reaction completely with HPLC (high-performance liquid chromatography), changing a dehydration device into an external negative-pressure microwave condensing device, setting distilling power, collecting fractions and cooling to obtain a light yellow crystalline solid that is 2(3H)-benzofuranone. The method provided by the invention is a process for synthesizing 2(3H)-benzofuranone, which has the advantages of simple operation, short production period, low energy consumption, no solvent and high yield, and being green and pollution-free.
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Description

technical field

[0001] This paper relates to the field of chemical synthesis, in particular to a method for synthesizing 2(3H)-benzofuranone by microwave. Background technique

[0002] Azoxystrobin is a methoxyacrylic fungicide developed by Syngenta, and currently ranks first in sales of fungicides, and 2(3H)-benzofuranone is a key intermediate of the fungicide azoxystrobin. At present, the main synthetic methods at home and abroad use o-chlorophenylacetic acid or o-bromophenylacetic acid, or o-iodophenylacetic acid as starting materials, after high temperature and high pressure reaction, acidification, solvent extraction, and crystallization to obtain o-hydroxyphenylacetic acid. The rate is about 60%. Dissolve o-hydroxyphenylacetic acid with 3 to 4 times of toluene, then add sulfuric acid or p-toluenesulfonic acid as a dehydration catalyst, react at a high temperature of 110°C to 120°C for 8h to 12h, reflux and dehydrate, wash with water and remove toluene. Another solvent...

Claims

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