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Method for producing chlorpropham

A technology of chlorphenamine and chloroaniline, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbamic acid derivatives, etc., can solve problems such as no pretreatment of raw materials, need for distillation or rectification, poor product quality, etc. Achieve the effect of improving product quality, reducing production energy consumption, and less impurities

Active Publication Date: 2011-08-31
CAC NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis method used for chlorphenamine is mainly the isopropyl chloroformate method: that is, the condensation reaction is carried out with m-chloroaniline and isopropyl chloroformate, but the raw materials are not pretreated, and dilute acid is not used for neutralization at the end of the synthesis. Poor, distillation or rectification is required for qualified treatment, and there are defects such as high energy consumption and long cycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Bubble isopropyl chloroformate into an inert gas under a vacuum of -0.05Mpa, and perform bubbling degassing at 25°C for 2 hours;

[0022] (2) m-chloroaniline is preferred, and the content of isomers is controlled at 0.2%;

[0023] (3) Add 129g of m-chloroaniline to 400g of 14% liquid caustic soda, add 136g of treated isopropyl chloroformate dropwise under cooling conditions below 40°C, and keep warm for one hour at 60°C after dropping;

[0024] (4) Add 10% dilute hydrochloric acid dropwise to the reaction solution obtained in the above steps, adjust the pH value to 7, then add deionized water for water washing and stratification, the lower oil layer after stratification can obtain 214g of the crude product of chlorphenamine, after dehydration The finished product is 211g, the content is 99.3%, and the yield is 98.06%.

Embodiment 2

[0026] (1) Bubble isopropyl chloroformate into an inert gas under a vacuum of -0.09Mpa, and perform bubbling degassing at 30°C for 2 hours;

[0027] (2) m-chloroaniline is preferred, and the content of isomers is controlled at 0.1%;

[0028] (3) Add 129g of m-chloroaniline to 350g of 14% liquid caustic soda, add 130g of treated isopropyl chloroformate dropwise under cooling conditions below 40°C, and keep warm at 60°C for one hour after dropping;

[0029] (4) Add 60% dilute sulfuric acid dropwise to the reaction solution obtained in the above steps, adjust the pH value to 7, then add deionized water for water washing and stratification, the lower oil layer after stratification can obtain 213.5 g of the crude product of chlorphenamine, dehydrate The finished product is 210.5g, the content is 99.5%, and the yield is 98.03%.

Embodiment 3

[0031] (1) Bubble isopropyl chloroformate into an inert gas under a vacuum of -0.07Mpa, and perform bubbling degassing at 28°C for 2 hours;

[0032] (2) m-chloroaniline is preferred, and the content of isomers is controlled at 0.2%;

[0033] (3) Add 129g of m-chloroaniline to 400g of 14% liquid caustic soda, add 136g of treated isopropyl chloroformate dropwise under cooling conditions below 40°C, and keep warm at 60°C for one hour after dropping;

[0034] (4) Add 20% dilute hydrochloric acid dropwise to the reaction solution obtained in the above steps, adjust the pH value to 7, then add deionized water for water washing and stratification, the lower oil layer after stratification can obtain 214.5 g of the crude product of chlorphenamine, and dehydrate The finished product is 211g, the content is 99.4%, and the yield is 98.2%.

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Abstract

The invention discloses a method for producing chlorpropham, which comprises the following steps of: performing bubbling degassing treatment on isopropyl chlorocarbonate at the temperature of between 5 and 40DEG C under negative pressure condition; controlling content of isomerides of a raw material of m-chloroaniline to be within 0.2 percent, adding the m-chloroaniline into caustic soda liquid, and adding the treated isopropyl chlorocarbonate for reaction; regulating the PH value of reaction liquid to be 6-8 by using dilute acid, adding deionized water for washing and demixing, and obtaininga lower oil layer, namely a crude product of chlorpropham; and dehydrating the crude product to obtain the qualified product. By pretreating the raw material and acidifying synthetic liquid, the product quality is improved and production energy consumption is reduced.

Description

technical field [0001] The invention relates to a method for producing chlorphenamine. Background technique [0002] Chlorpropham (CIPC), the English common name is chlorpropham, the chemical name is 3-chloroaniline isopropyl formate, molecular formula: C 10 h 12 ClNO 2 , Chlorphenamine is a white crystal with a melting point of 38-41.5°C, hardly soluble in water, soluble in alcohols, aromatic hydrocarbons and most organic solvents, stable in environments below 100°C, and slowly hydrolyzed in acidic and alkaline media. [0003] At present, the synthesis method used for chlorphenamine is mainly the isopropyl chloroformate method: that is, the condensation reaction is carried out with m-chloroaniline and isopropyl chloroformate, but the raw materials are not pretreated, and dilute acid is not used for neutralization at the end of the synthesis. Poor, qualified treatment requires distillation or rectification, which has defects such as high energy consumption and long cycle....

Claims

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Application Information

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IPC IPC(8): C07C271/28C07C269/04
Inventor 谢思勉卞进平王海水刘兴华吴学丹
Owner CAC NANTONG CHEM
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