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Synthetic method of propyzamide

A synthetic method, the technology of pentynclochlor, which is applied in the field of synthesis of pentynclod, can solve the problems of harsh production environment, high cost of raw materials, long reaction time, etc., and achieve improved process safety, low production cost and simple operation Effect

Active Publication Date: 2015-03-25
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the above two methods, 3,5-diaminotoluene is used as raw material, which has high raw material cost, low yield, large pollution and harsh production environment
The method of using anthranilic acid as the starting material is more economical, but this method has the disadvantages of long reaction time and cumbersome operation, especially in the process of synthesizing 3,5-dichlorobenzoic acid, the risk of diazotization process is high

Method used

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  • Synthetic method of propyzamide
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 300g of chloroform and 100g of ethanol to 100.0g of benzonitrile (content 99%), and then add 1209.4g of sodium hypochlorite (content 13%), use 37% hydrochloric acid to keep the pH of the system at 3.0-4.0, at 55-60 At ℃, react until the content of 3,5-dichlorobenzonitrile is 99.5%, then add 30% sodium hydroxide under normal pressure to keep the pH value of the reaction system at 12-13, and keep the reaction at 80-90℃ After 2.5 hours, acidify the system with 37% hydrochloric acid until the pH value of the system is 1.0, react at 50-60°C for 1.0h, filter again, and dry at 90-110°C to obtain 182.5g of 3, with a content of 99.0%. 5-Dichlorobenzoic acid.

[0037] Take 100g of the obtained 3,5-dichlorobenzoic acid and mix it with 74.7g of thionyl chloride (content 99%), reflux at 70-80°C for 2.0h, and then recover the chlorine at normal pressure and 75-82°C sulfoxide, and then distill 3,5-dichlorobenzoyl chloride at 185-195°C and -0.01MPa for the next reaction.

[0038]...

Embodiment 2

[0040] Add 1500g chloroform and 500g ethanol to 100.0g benzonitrile (content 99%) respectively, then add 1209.4g sodium hypochlorite (content 13%), use 98% sulfuric acid to keep the pH value of the system at 5.0-6.0, at 60-70 At ℃, react until the content of 3,5-dichlorobenzonitrile is 99.4%, and then add 20% sodium hydroxide under normal pressure to keep the pH value of the reaction system at 11-12, and keep the reaction at 80-90℃ After 3.0 hours, acidify the system with 37% hydrochloric acid until the pH value of the system is 0, react at 50-60°C for 0.5h, filter again, and dry at 90-110°C to obtain 182.5g of 3, with a content of 99.0%. 5-Dichlorobenzoic acid.

[0041] Take 100g of the obtained 3,5-dichlorobenzoic acid and mix it with 74.7g of thionyl chloride (content 99%), reflux at 70-80°C for 2.5h, and then recover at normal pressure and 75-82°C Thionyl chloride, then distill 3,5-dichlorobenzoyl chloride at 185-195°C and -0.05MPa for the next reaction.

[0042] Take 52...

Embodiment 3

[0044] Add 75g of chloroform and 25g of ethanol to 100.0g of benzonitrile (content 99%), and then add 1209.4g of sodium hypochlorite (content 13%), use 25% hydrochloric acid to keep the pH value of the system at 0-1.0, at 55-70 At ℃, react until the content of 3,5-dichlorobenzonitrile is 99.5%, then add 10% sodium hydroxide under normal pressure to keep the pH value of the reaction system at 13-14, and keep the reaction at 80-90℃ After 2.7 hours, acidify the system with 37% hydrochloric acid until the pH value of the system is 1.5, react at 50-60°C for 0.6h, filter again, and dry at 90-110°C to obtain 182.3g of 3, with a content of 99.0%. 5-Dichlorobenzoic acid.

[0045] Mix 100g of the obtained 3,5-dichlorobenzoic acid with 74.7g of thionyl chloride (content 99%), reflux at 70-80°C for 3.0h, and then recover chlorine at normal pressure and 75-82°C sulfoxide, and then distill 3,5-dichlorobenzoyl chloride at 185-195°C and -0.15MPa for the next reaction.

[0046] Take 52.8g of...

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Abstract

The invention discloses a synthetic method of propyzamide. The method comprises the following steps: by taking 3, 5-dichlorobenzoic acid as a raw material, chlorinating 3, 5-dichlorobenzoic acid to generate 3, 5-dichlorobenzoyl chloride; further performing reaction between generated 3, 5-dichlorobenzoyl chloride and 3-amino-3-methyl butyne in the presence of alkaline matters and solvents; and filtering, drying and recrystallizing the reaction solution to obtain propyzamide. The material in the process is easy to obtain and low in cost, the production cost of products is low, and the safety coefficient of the process is high. The method is simple to operate, short in process flow and beneficial for industrialized production, and is a novel process for synthesizing propyzamide.

Description

technical field [0001] The invention relates to a new method for synthesizing pentynclod, in particular to a method for synthesizing pentynclod with 3,5-dichlorobenzoic acid as a starting material. Background technique [0002] Penpyramide, commercially known as propanil, is a widely used amide herbicide, commonly used for the control of broadleaf weeds. At present, only Dow AgroSciences of the United States produces 98% of pentynchlor, while other countries produce 94-95%. The sales of pentynchlor technical have been stable in the past ten years, and the market prospect is good. [0003] The currently reported synthetic method of pentynchloride mainly involves the acylation of 3,5-dichlorobenzoic acid to obtain 3,5-dichlorobenzoyl chloride, and then the 3,5-dichlorobenzoyl chloride is combined with 3-amino- 3-Methylbutyne reaction system. [0004] Wherein 3,5-dichlorobenzoic acid synthetic method has following two kinds according to raw material classification: [0005] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/65C07C231/02C07C63/70C07C51/02C07C51/08
Inventor 孙国庆侯永生姚红霞邹宗加李志清李宗清王庆伟
Owner SHANDONG WEIFANG RAINBOW CHEM
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