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Synthesis method of optically active metalaxyl

A synthetic method, the technology of metalaxyl, applied in the field of synthesis of optically active metalaxyl, can solve the problems of low total yield, environmental pollution, low yield, etc., and achieve the reduction of three wastes, product yield and yield High and simplified operation steps

Inactive Publication Date: 2019-01-11
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since this method does not need to be split to obtain the target product with higher optical purity, it is a better method because of its high economic efficiency. This process will produce a large amount of sulfur dioxide and hydrogen chloride waste gas, which will pollute the environment, and the total cost of the second step The yield is only 68.5%, which is low

Method used

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  • Synthesis method of optically active metalaxyl
  • Synthesis method of optically active metalaxyl
  • Synthesis method of optically active metalaxyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of synthetic method of optically active metalaxyl

[0033] Optically active metalaxyl, synthesized by the following method:

[0034] Step S10, add 200kg of methanol and 190kg (2kmol) of chloroacetic acid into a 3000L reaction kettle, start stirring, and heat up until the materials are basically dissolved, then add 790kg (4.1kmol) of 28% sodium methoxide, heat up to 58°C, and keep warm for 0.5 hour, the reaction is over, methanol is recovered under reduced pressure, the temperature is at 80°C, and the vacuum degree is 0.098Mpa;

[0035] Step S20, after the decompression is completed, the temperature is lowered to 35°C, 1800kg of toluene is added, 94.4kg (0.68kmol) of phosphorus trichloride is added dropwise at 40°C, the addition is completed in 35 minutes, and the temperature is kept at 50°C for 1.2 hours;

[0036] Step S30, after the heat preservation is completed, the tail gas absorption device is turned on, and 393kg (95%, 1.8kmol) of D-N-(2,6-dimethylphenyl)a...

Embodiment 2

[0042] A kind of synthetic method of optically active metalaxyl

[0043] Optically active metalaxyl, synthesized by the following method:

[0044] Step S10, add 300kg of methanol and 190kg (2kmol) of chloroacetic acid into a 3000L reaction kettle, start stirring, and heat up until the materials are basically dissolved, then add 790kg (4.1kmol) of 28% sodium methoxide, heat up to 65°C, and keep warm for 1 hour, the reaction is over, methanol is recovered under reduced pressure, the temperature is 75°C, and the vacuum is 0.098Mpa;

[0045] Step S20, after the decompression is completed, the temperature is lowered to 40°C, 1300kg of toluene is added, 105.6kg (0.76kmol) of phosphorus trichloride is added dropwise at 45°C, the addition is completed in 45 minutes, and the temperature is kept at 40°C for 0.8 hours;

[0046] Step S30, after the heat preservation is completed, the tail gas absorption device is turned on, and 436 kg (95%, 2.0 kmol) of D-N-(2,6-dimethylphenyl)alanine me...

Embodiment 3

[0052] A kind of synthetic method of optically active metalaxyl

[0053] Optically active metalaxyl, synthesized by the following method:

[0054] Step S10, add 300kg of methanol and 190kg (2kmol) of chloroacetic acid into a 3000L reaction kettle, start stirring, heat up until the materials are basically dissolved, add 732kg (3.8kmol) of 28% sodium methoxide, heat up to 60°C, and keep warm for 1.2 hour, the reaction is over, methanol is recovered under reduced pressure, the temperature is at 72°C, and the vacuum degree is 0.098Mpa;

[0055] Step S20, after the decompression is completed, the temperature is lowered to 38°C, 1600kg of toluene is added, 83.3kg (0.6kmol) of phosphorus trichloride is added dropwise at 43°C, and the addition is completed in 25 minutes, and the temperature is kept at 60°C for 0.5 hours;

[0056] Step S30, after the heat preservation is completed, the tail gas absorption device is turned on, and 427 kg (95%, 1.96 kmol) of D-N-(2,6-dimethylphenyl)alan...

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Abstract

The invention discloses a synthesis method of optically active metalaxyl. The optically active metalaxyl is synthesized by performing methoxylation and acylating chlorination on chloroacetic acid to obtain methoxyacetyl chloride and then reacting Methoxyacetyl chloride with D-N-(2,6-dimethylphenyl) alanine methyl ester; a one-pot method operation is adopted for the synthesis; the two-step reactionof methoxylation and acylating chlorination is directly used for a next-step reaction without post-treatment. According to the process of the optically active metalaxyl, by adopting the one-pot method operation, the operation steps are simplified, the production of three wastes is decreased, the synthesis cost is reduced, the obtained product is stable in quality and relatively high in output andyield, and the synthesis method is suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of bactericidal active compounds, in particular to a method for synthesizing optically active metalaxyl. Background technique [0002] Metalaxyl (racemate) pesticide is a mixture composed of equal amounts of R isomer and S isomer. The current annual market output is more than 20,000 tons, far exceeding other types of fungicides. One of the last major fungicide varieties. The bactericidal effect of metalaxyl is mainly the R isomer, that is, optically active metalaxyl, but because of the existence of the S isomer, the bactericidal effect of the product is greatly reduced, resulting in a great increase in the dosage per unit. Studies have shown that optically active metalaxyl has the characteristics of low toxicity, safety, environmental protection, and greenness compared with spheroid metalaxyl, and optically active metalaxyl has higher bactericidal activity than racemate, and its bactericidal activity is hig...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C235/16
CPCC07B2200/07C07C227/02C07C231/02C07C303/26C07C309/73C07C229/18C07C235/16
Inventor 李冬良潘光飞王进李成斌
Owner 浙江禾本科技股份有限公司
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