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Synthesis method of metalaxyl key intermediate N-(2, 6-dimethylphenyl) amino methyl propionate

A technology of methylalanine and xylyl, which is applied in the field of synthesis of N-methylalanine, a key intermediate of metalaxyl, can solve the problem that the product must be rectified, the synthesis reaction temperature is high, and the intermediate is recovered Difficulties and other problems, to achieve the effect of saving energy consumption, increasing reaction yield and reducing production efficiency

Active Publication Date: 2022-02-11
浙江禾本科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The method for synthesizing methyl N-(2,6-xylyl)aminopropionate by old technology has high synthetic reaction temperature, low yield of crude product, long reaction time, complicated operation steps, and the product must be rectified. Problems such as difficulty in recycling

Method used

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  • Synthesis method of metalaxyl key intermediate N-(2, 6-dimethylphenyl) amino methyl propionate
  • Synthesis method of metalaxyl key intermediate N-(2, 6-dimethylphenyl) amino methyl propionate

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Embodiment 1

[0029] A kind of synthetic method of metalaxyl key intermediate N-(2,6-xylyl)alanine methyl ester

[0030] Metalaxyl key intermediate N-(2,6-xylyl)alanine methyl ester is prepared by the following synthetic method:

[0031] The reaction equation is as follows:

[0032]

[0033] Add 495g of methyl chloropropionate, 563g of 2,6-dimethylaniline, 245g of sodium carbonate, and 16g of potassium iodide into a four-necked flask, and raise the temperature to 55°C for 16 hours under ultrasonic waves; Control the content of methyl chloropropionate to be less than 6.6% in the process, add the deionized water of 566g, wash layering, obtain the crude product of N-(2,6-xylyl) methyl aminopropionate; Distill under reduced pressure under vacuum 24.6g of the previous fraction 2,6-dimethylaniline (containing 6.3g of N-(2,6-xylyl)aminopropionate methyl ester) was distilled, which was applied to the next batch of reactions, and then N-(2 ,6-xylyl)aminopropionic acid methyl ester 775.6g, conte...

Embodiment 2

[0035] A kind of synthetic method of metalaxyl key intermediate N-(2,6-xylyl)alanine methyl ester

[0036] Metalaxyl key intermediate N-(2,6-xylyl)aminopropionate methyl ester is prepared by the following synthetic method: 495g of methyl chloropropionate, 516g of 2,6-dimethylaniline, 246g of Sodium carbonate and 16g of potassium iodide were added to a four-necked flask, and under ultrasonic waves, the temperature was raised to 66°C for 6 hours of heat preservation reaction; during the heat preservation reaction, the content of methyl chloropropionate was controlled to be less than 6.5%, and 566g of deionized water was added, washed with water Layered to obtain the crude product of N-(2,6-xylyl)aminopropionic acid methyl ester; Distillation under reduced pressure under vacuum, steaming out the front fraction 2,6-dimethylaniline 25.5g (which contains N-(2, 5.5 g of methyl 6-xylyl)alanine), applied mechanically to the next batch of reactions, and then distilled 616 g of methyl N-...

Embodiment 3

[0038] A kind of synthetic method of metalaxyl key intermediate N-(2,6-xylyl)alanine methyl ester

[0039] Metalaxyl key intermediate N-(2,6-xylyl)aminopropionate methyl ester is prepared by the following synthetic method: 495g of methyl chloropropionate, 516g of 2,6-dimethylaniline, 225g of Add sodium carbonate and 11g of potassium iodide into a four-neck flask, raise the temperature to 66°C for 6 hours under ultrasonic waves, and keep the temperature for 6 hours; control the content of methyl chloropropionate to less than 6.5% during the heat preservation reaction, add 566g of deionized water, wash with water Layered to obtain the crude product of N-(2,6-xylyl)aminopropionic acid methyl ester; Distillation under reduced pressure under vacuum, steaming out the front fraction 2,6-dimethylaniline 41.2g (which contains N-(2, 6-xylyl)alanine methyl ester 16.3g), applied mechanically to the next batch of reactions, and then distilled N-(2,6-xylyl)alanine methyl ester 795g, content...

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Abstract

The invention discloses a synthesis method of a metalaxyl key intermediate N-(2, 6-dimethylphenyl) amino methyl propionate. The method comprises the following steps: by taking methyl chloropropionate and 2, 6-dimethylaniline as raw materials, sodium carbonate as an acid-binding agent and potassium iodide as a catalyst, raising the temperature to 66-666 DEG C under ultrasonic waves, carrying out heat preservation reaction for 6-612 hours, washing with water, and layering to obtain the N-(2, 6-dimethylphenyl) amino methyl propionate crude product, and carrying out vacuum reduced pressure distillation to obtain the N-(2, 6-dimethylphenyl) amino methyl propionate. The content of the N-(2, 6-dimethylphenyl) amino methyl propionate finally prepared by the reaction is greater than 96.2%, and the yield is greater than 96.3%.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing methylalaxyl key intermediate N-(2,6-xylyl)alanine. Background technique [0002] Metalaxyl is a high-efficiency, low-toxic systemic fungicide with protective and therapeutic effects. It mainly works by inhibiting the protein synthesis of Oomycete fungi. The chemical name is N-(2,6-xylyl) -N(2-Methoxyacetyl-rac-methyl-alanine). The synthesis method of N-(2,6-xylyl)-N(2-methoxyacetyl-racemic-alanine) mainly uses N-(2,6-xylyl)alanine It can be prepared by amidation reaction between methyl ester and methoxyacetyl chloride. Among them, methyl N-(2,6-xylyl)alanine is one of the most important reactants for the synthesis of metalaxyl, and is the most critical intermediate of metalaxyl. [0003] The synthesis of methyl N-(2,6-xylyl)alanine generally uses 2,6-dimethylaniline and methyl chloropropionate as raw materials, sodium carbonate as an acid-b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/08C07C227/40C07C229/18
CPCC07C227/08C07C227/40C07C229/18
Inventor 赵振东潘光飞张卫明王进徐瑶曾挺
Owner 浙江禾本科技股份有限公司
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