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Method for preparing chlorophenylglycine

A technology of p-chlorophenylglycine and p-chlorobenzaldehyde, which is applied to the preparation of cyanide reaction, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of long reaction time period, difficult process control, and low product yield, etc. problems, to achieve fast response, ensure the safety of production operations, and simple equipment

Active Publication Date: 2016-11-09
内蒙古诚信永安化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because these two commonly used methods mainly adopt the kettle-type intermittent production process, the reaction time period is long, about 8-9h; the process control is difficult, the product yield is not high, the equipment investment is large, and the operation is cumbersome

Method used

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  • Method for preparing chlorophenylglycine
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A. Preparation of p-chlorophenylhydantoin

[0034] a) Preparation of raw materials: prepare p-chlorobenzaldehyde feed solution, 20% ammonium bicarbonate solution, 30% sodium cyanide solution and 30% sodium hydroxide solution that melt into liquid;

[0035] b) After the p-chlorobenzaldehyde is heated and melted into a liquid state, it is passed into the G1R*F module of the preheating zone pipeline 1 via a metering pump, the control flow is 5.0g / min, and the preheating temperature of the G1R*F module is 50℃;

[0036] The 20% ammonium bicarbonate aqueous solution and the 30% sodium cyanide solution are respectively fed into the G1SHH module of the preheating zone pipeline 1 through the metering pump to preheat and mix, and the flow rate of the 20% ammonium bicarbonate aqueous solution is controlled to 21.0g / min. The flow rate of 30% sodium cyanide solution is 5.8g / min, and the preheating temperature of G1SHH module is 50℃;

[0037] c) The p-chlorobenzaldehyde feed solution preheat...

Embodiment 2

[0047] A. Preparation of p-chlorophenylhydantoin

[0048] a) Preparation of raw materials: prepare p-chlorobenzaldehyde feed solution, 20% ammonium bicarbonate solution, 30% sodium cyanide solution and 30% sodium hydroxide solution that melt into liquid;

[0049] b) After the p-chlorobenzaldehyde is heated and melted into a liquid state, it is passed into the G1R*F module of the preheating zone pipeline 1 through a metering pump, the control flow is 7.5g / min, and the preheating temperature of the G1R*F module is 55℃;

[0050] The 20% ammonium bicarbonate aqueous solution and the 30% sodium cyanide solution are respectively fed into the G1SHH module of the preheating zone pipeline 1 through the metering pump to preheat and mix, and the flow rate of the 20% ammonium bicarbonate aqueous solution is controlled to 35.9g / min. The flow rate of 30% sodium cyanide solution is 11.3g / min, and the preheating temperature of G1SHH is 55℃;

[0051] c) The p-chlorobenzaldehyde feed solution preheated...

Embodiment 3

[0061] A. Preparation of p-chlorophenylhydantoin

[0062] a) Preparation of raw materials: preparation of p-chlorobenzaldehyde feed solution, 20% ammonium bicarbonate solution, 30% sodium cyanide solution and 30% sodium hydroxide solution that melt into liquid;

[0063] b) After the p-chlorobenzaldehyde is heated and melted into a liquid state, it is fed into the G1R*F module in the preheating zone pipeline 1 via a metering pump, and the control flow is 10.0g / min, and the preheating temperature of the G1R*F module is 60℃;

[0064] Pass the 20% ammonium bicarbonate aqueous solution and 30% sodium cyanide solution through the metering pump into the G1SHH module in the preheating zone pipeline 1 to preheat and mix, and control the flow rate of the 20% ammonium bicarbonate aqueous solution to 56.3g / min , The flow rate of 30% sodium cyanide solution is 17.4g / min, and the preheating temperature of G1SHH is 60℃;

[0065] c) The p-chlorobenzaldehyde feed solution preheated in step a) and the ...

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Abstract

The invention relates to a method for preparing chlorophenylglycine. The method is characterized in that p-chlorobenzaldehyde, ammonium bicarbonate and sodium cyanide are subjected to a complete reaction in a micro-channel reactor, and a tubular-type reactor is used for preparing the chlorophenylglycine. According to the invention, the raw materials are subjected to cyclization in the micro-channel reactor through a flow counter to prepare an intermediate p-chlorophenylhydantoin, alkaline hydrolysis is carried out on the intermediate through the tubular-type reactor by the flow counter to prepare the chlorophenylglycine, the reaction is complete in 8-18 minutes, and the chlorophenylglycine is introduced into a reaction bottle and is subjected to acidifying crystallization. The product purity is 98.0% and above, and the yield is 95% and above. The method has the advantages of concise technical route and fast reaction speed, can increase the work efficiency and production capacity, and can ensure the production and operation security of the processes.

Description

Technical field [0001] The invention relates to a preparation method of p-chlorophenylglycine, which is an intermediate of medicines and pesticides, in particular to a method for preparing chlorophenylglycine. Background technique [0002] P-Chlorophenylglycine is an important organic intermediate and an important intermediate of the pesticide arylpyrrole nitrile insecticide and acaricide bromipronil. [0003] At present, there are many methods for preparing p-chlorophenylglycine in China, mainly using the "Bucherer-Bergs method". Bucherer-Bergs reaction is a direct reaction of carbonyl compounds with potassium cyanide and ammonium carbonate, or cyanohydrin and ammonium carbonate to form hydantoins. Compound reaction. That is, p-chlorobenzaldehyde is used as a raw material to react with ammonium bicarbonate and sodium cyanide to prepare a p-chlorophenylhydantoin intermediate, and then an alkaline hydrolysis reaction to obtain mixed-rotation p-chlorophenylglycine, such as patent CN...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/24C07C229/36
CPCC07C227/24C07D233/76C07C229/36
Inventor 刘少华石会王晓龙郭亚运张静
Owner 内蒙古诚信永安化工有限公司
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