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Synthesis method of 3-isochromanone

A synthesis method and technology of isochromone, applied in the direction of organic chemistry, etc., can solve the problems of restricting industrialized large-scale production, long reaction time, low conversion rate, etc. The effect of low production cost

Pending Publication Date: 2020-12-25
NINGXIA SIKEDA BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From bibliographical reports, its existing synthesis method has the following deficiencies, such as harsh conditions, higher cost, difficult operation, low conversion rate, long reaction time, and low yield etc.
This greatly restricts its industrial mass production

Method used

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  • Synthesis method of 3-isochromanone
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  • Synthesis method of 3-isochromanone

Examples

Experimental program
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preparation example Construction

[0032] The synthetic method of 3-isochromone of the present invention comprises the steps:

[0033] (1) take o-xylene as raw material to synthesize o-methyl benzyl chloride, and the reaction equation is as follows:

[0034]

[0035] (2) take o-methyl benzyl chloride as raw material to synthesize o-toluene acetonitrile, and the reaction equation is as follows:

[0036]

[0037] (3) take o-toluene acetonitrile as raw material to synthesize sodium o-toluene acetate, reaction equation is as follows:

[0038]

[0039] (4) take sodium o-toluene acetate as raw material to synthesize o-toluene acetic acid, and the reaction equation is as follows:

[0040]

[0041] (5) take o-methylphenylacetic acid as raw material synthetic 2-chloromethylphenylacetic acid, reaction equation is as follows:

[0042]

[0043] (6) take 2-chloromethylphenylacetic acid as raw material synthetic 3-isochromone, and reaction equation is as follows:

[0044]

Embodiment 1

[0046] The synthetic method of 3-isochromone described in the present embodiment comprises the steps:

[0047] (1) take o-xylene as raw material to synthesize o-methyl benzyl chloride;

[0048] The concrete process of step (1) is in 3000 liters of reaction flasks, first adds 2332g (22mol) o-xylene and heats up to 100 ℃, then passes into 781g (11mol) chlorine gas, reacts 5h under the effect of light source, the wavelength of light source Select at 2500nm to obtain o-methylbenzyl chloride, and then carry out rectification and purification on the obtained o-methylbenzyl chloride to obtain o-methylbenzyl chloride with a purity of more than 99%.

[0049] (2) take o-methyl benzyl chloride as raw material to synthesize o-toluene acetonitrile;

[0050] The concrete process of step (2) is in 3000 liters of reaction bottles, add the aqueous solution 1960g (wherein sodium cyanide is 12mol) of the sodium cyanide of 30% by mass percentage, be warming up to 100 ℃, dropwise add o-methyl ben...

Embodiment 2

[0060] The synthetic method of 3-isochromone described in the present embodiment comprises the steps:

[0061] (1) take o-xylene as raw material to synthesize o-methyl benzyl chloride;

[0062] The specific process of step (1) is to add 2332g (22mol) o-xylene to 95°C at first in a 3000-liter reaction bottle, then feed 937.2g (13.2mol) chlorine gas, and react for 4 hours under the action of a light source. The wavelength is selected at 3000nm to obtain o-methylbenzyl chloride, and then the obtained o-methylbenzyl chloride is subjected to rectification and purification to obtain o-methylbenzyl chloride with a purity of more than 99%.

[0063] (2) take o-methyl benzyl chloride as raw material to synthesize o-toluene acetonitrile;

[0064] The concrete process of step (2) is in 3000 liters of reaction bottles, add the aqueous solution 2352g (wherein sodium cyanide is 12mol) of the sodium cyanide of 25% by mass percent, be warming up to 30 ℃, dropwise add o-methyl benzyl chloride ...

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Abstract

The invention belongs to the technical field of synthesis of organic intermediates, and particularly relates to a synthesis method of 3-isochromanone, which comprises the following steps of: (1) synthesizing o-methyl benzyl chloride by using o-xylene as a raw material; (2) synthesizing o-methyl benzyl cyanide by taking o-methyl benzyl chloride as a raw material; (3) synthesizing sodium o-methyl phenylacetate by taking o-methyl benzyl cyanide as a raw material; (4) synthesizing o-methyl phenylacetic acid by taking sodium o-methyl phenylacetate as a raw material; (5) synthesizing 2-chloromethylphenylacetic acid by taking o-methyl phenylacetic acid as a raw material; and (6) synthesizing 3-isochromanone by taking 2-chloromethyl phenylacetic acid as a raw material. The synthesis method of 3-isochromanone has the advantages of simple reaction process, easily available raw materials, mild reaction conditions, high product yield, low production cost, high yield, high product purity, good quality, low production waste discharge amount and the like, the product purity is greater than or equal to 99.5%, the production yield is greater than or equal to 92%, and the product meets the use requirements of foreign high-end users.

Description

technical field [0001] The invention belongs to the technical field of synthesis of organic intermediates, and in particular relates to a synthesis method of 3-isochromone. Background technique [0002] Compared with triazole fungicides, methoxyacrylate fungicides come from behind. In 2016, with a total sales of US$3.396 billion and an advantage gap of US$421 million, this type of product fixed the old triazole fungicides in the second place in the global fungicide market. Among the top 15 fungicides in the world, methoxyacrylate fungicides occupy 3 seats, and azoxystrobin, pyraclostrobin and picoxystrobin made a big appearance. [0003] Azoxystrobin is not only the leader in the global fungicide market, but also the largest product in the rice fungicide market. In 2016, the top three products in the rice fungicide market were: azoxystrobin, tricyclazole and difenoconazole, and their sales in rice were: 118 million, 110 million and 56 million US dollars. Under the leaders...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/76
CPCC07D311/76
Inventor 田永富钱云祥张康刘小洲
Owner NINGXIA SIKEDA BIOTECH CO LTD
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