Synthetic process of 2,4-dichloro-5-isopropoxyl phenyl hydrazine

A technology of isopropoxyphenylhydrazine and a synthesis method, which is applied in the fields of hydrazine preparation, organic chemistry and the like, can solve the problems of high equipment requirements, large waste discharge, low yield and the like, and achieves low equipment requirements and waste. The effect of less emission and easy control of the reaction

Inactive Publication Date: 2017-08-11
重庆锦杉科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis methods of 2,4-dichloro-5-isopropoxyphenylhydrazine cannot avoid operations such as diazotization, reduction, acidification, and alkali analysis of 2,4-dichloro-5-isopropoxyaniline , these operations have strict requirements on the reaction temperature, diazotization and reduction reactions must be carried out at low temperature, and the addition rate of sodium nitrite solution and the degree of reaction are not well controlled, and side reactions will occur and lead to the generation of by-products. will affect the following reduction reaction
The process route using sodium sulfite or sodium bisulfite as a reducing agent is relatively mature and has been widely used in the industrial production of 2,4-dichloro-5-isopropoxyphenylhydrazine, but its control conditions are many and the process is complicated. The operation is cumbersome, if you need to use sodium hydroxide solution to adjust the pH value to 6.5~7, if the control is not good, there will be asphalt-like by-products, and the reaction temperature needs to be adjusted many times during the whole process
When stannous chloride is used as reducing agent, not only the price is relative

Method used

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  • Synthetic process of 2,4-dichloro-5-isopropoxyl phenyl hydrazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Put 220g of 2,4-dichloro-5-isopropoxyaniline and 168g of acetonazine into a four-neck flask with stirring, dropping funnel, thermometer and rectification column, and the upper part of the receiver of the rectification column is connected to a Conduit to absorb ammonia gas; start stirring, heat the solution to 120-130°C, slowly add 54ml of water dropwise into the four-necked flask, control the reaction temperature at 100°C-130°C, when the gas generated by the reaction enters the rectification column Finally, extract acetone and recover ammonia at the column top temperature of 54°C to 58°C. The water vapor and acetonazine entering the rectification column are condensed and flow back to the flask to continue to participate in the reaction; When no ammonia gas is released from the receiver of the rectifying column, the reaction ends, and all the water and acetonazine in the flask are evaporated with negative pressure. The solid matter in the flask is washed with absolute eth...

Embodiment 2

[0014] Put 220g of 2,4-dichloro-5-isopropoxyaniline and 196g of acetonazine into a four-neck flask with stirring, dropping funnel, thermometer and rectification column, and the receiver of the rectification column is connected to a Conduit to absorb ammonia gas; start stirring, heat the solution to 120-130°C, slowly add 63ml of water into the four-neck flask dropwise, control the reaction temperature at 100°C-130°C, when the gas generated by the reaction enters the rectification column Finally, extract acetone and recover ammonia at the column top temperature of 54°C to 58°C. The water vapor and acetonazine entering the rectification column are condensed and flow back to the flask to continue to participate in the reaction; When no ammonia gas is released from the receiver of the rectifying column, the reaction ends, and all the water and acetonazine in the flask are evaporated with negative pressure. The solid matter in the flask is washed with absolute ethanol and dried to ob...

Embodiment 3

[0016] Put 220g of 2,4-dichloro-5-isopropoxyaniline and 224g of acetonazine into a four-neck flask with stirring, dropping funnel, thermometer and rectification column. Conduit to absorb ammonia gas; start stirring, heat the solution to 120-130°C, slowly add 72ml of water dropwise into the four-neck flask, control the reaction temperature at 100°C-130°C, when the gas generated by the reaction enters the rectification column Finally, extract acetone and recover ammonia at the column top temperature of 54°C to 58°C. The water vapor and acetonazine entering the rectification column are condensed and flow back to the flask to continue to participate in the reaction; When no ammonia gas is released from the receiver of the rectifying column, the reaction ends, and all the water and acetonazine in the flask are evaporated with negative pressure. The solid matter in the flask is washed with absolute ethanol and dried to obtain 2,4-dichloro - 227.2 g of 5-isopropoxyphenylhydrazine.

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Abstract

The invention provides a synthetic process of 2,4-dichloro-5-isopropoxyl phenyl hydrazine. According to the method, 2,4-dichloro-5-isopropoxyl aniline, ketazine and water are used as raw materials, and the 2,4-dichloro-5-isopropoxyl phenyl hydrazine is synthesized through reaction at a certain temperature. Excessive ketazine and water are added in the reaction process to make the 2,4-dichloro-5-isopropoxyl aniline completely react in a reaction system, reduced pressure distillation is adopted to remove the water and the ketazine after reaction is completed, and a solid substance is washed and dried to obtain the 2,4-dichloro-5-isopropoxyl phenyl hydrazine. Compared with a traditional diazo-reaction process for synthesizing the 2,4-dichloro-5-isopropoxyl phenyl hydrazine, the process includes few reaction steps and is simple, the device requirements are not high, reaction is easy to control, the yield is high, the production process is low, waste discharge is little, and the process is a green and environment-friendly production process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of 2,4-dichloro-5-isopropoxyphenylhydrazine. Background technique [0002] 2,4-Dichloro-5-isopropoxyphenylhydrazine is an important intermediate for the synthesis of the pesticide oxadiazone, and also an intermediate for the synthesis of various medicines and pesticides, and has wide application value. [0003] At present, the synthesis methods of 2,4-dichloro-5-isopropoxyphenylhydrazine cannot avoid operations such as diazotization, reduction, acidification, and alkali analysis of 2,4-dichloro-5-isopropoxyaniline , these operations have strict requirements on the reaction temperature, diazotization and reduction reactions must be carried out at low temperature, and the addition rate of sodium nitrite solution and the degree of reaction are not well controlled, and side reactions will occur and lead to the generation of by-products. It w...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/22
CPCC07C241/02C07C243/22
Inventor 王伟
Owner 重庆锦杉科技有限公司
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