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A kind of method for preparing p-chlorophenylglycine

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

Active Publication Date: 2018-06-26
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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  • A kind of method for preparing p-chlorophenylglycine
  • A kind of method for preparing p-chlorophenylglycine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A. Preparation of p-chlorophenylhydantoin

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

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

[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 be 21.0g / min. The flow rate of 30% sodium cyanide solution is 5.8g / min, and the preheating temperature of the G1SHH module is 50°C;

[0037] c) The p-chlor...

Embodiment 2

[0047] A. Preparation of p-chlorophenylhydantoin

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

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

[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 be 35.9g / min. The flow rate of 30% sodium cyanide solution is 11.3g / min, and the preheating temperature of G1SHH is 55°C;

[0051] c) step a) preheated p-ch...

Embodiment 3

[0061] A. Preparation of p-chlorophenylhydantoin

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

[0063] b) After p-chlorobenzaldehyde is heated and melted into a liquid state, it is passed into the G1R*F module in the pipeline 1 of the preheating zone through the metering pump, and the flow rate is controlled at 10.0g / min, and the preheating temperature of the G1R*F module is 60°C;

[0064] 20% ammonium bicarbonate aqueous solution and 30% sodium cyanide solution are respectively passed through metering pumps to the G1SHH module in the preheating zone pipeline 1 to preheat and mix, and the flow rate of 20% ammonium bicarbonate aqueous solution is controlled to be 56.3g / min , the flow rate of 30% sodium cyanide solution is 17.4g / min, and the preheating temperature of G1SHH is 60°C;

[0065] c) The p-chlorobenzaldehyde fe...

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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 method for preparing medicine and pesticide intermediate p-chlorophenylglycine, in particular to a method for preparing chlorophenylglycine. Background technique [0002] p-Chlorphenylglycine is an important organic intermediate, and it is an important intermediate of the pesticide arylpyrrole nitrile insecticide and acaricide chlorfenapyr. [0003] At present, there are many methods for preparing p-chlorophenylglycine in China, mainly using the "Bucherer-Bergs method", Bucherer-Bergs reaction, which is the direct reaction of carbonyl compounds with potassium cyanide and ammonium carbonate, or cyanohydrin and ammonium carbonate to generate hydantoins The reaction of the compound. That is, p-chlorobenzaldehyde is used as a raw material, reacted with ammonium bicarbonate and sodium cyanide to prepare p-chlorophenylhydantoin intermediate, and then alkaline hydrolyzed to obtain mixed-rotated p-chlorophenylglycine, such as patent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/24C07C229/36
CPCC07C227/24C07D233/76C07C229/36
Inventor 刘少华申世刚王晓龙郭亚运张辰亮
Owner 内蒙古诚信永安化工有限公司
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