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Metamifop intermediate and preparation method of metamifop

A technology of fenpyramid and fenpyral, which is applied in the field of preparation of fenpyral herbicides, can solve problems such as high production cost and unsatisfactory waste liquid treatment, and achieve reduction of decomposition and reduction of raw materials cost and waste water treatment cost, and the effect of improving the yield

Inactive Publication Date: 2021-02-26
宁夏蓝田农业开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, due to the unsatisfactory treatment of waste liquid in the late stage of the system of DMF and water, the production cost is high

Method used

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  • Metamifop intermediate and preparation method of metamifop
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  • Metamifop intermediate and preparation method of metamifop

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preparation example Construction

[0034] Please refer to the attached figure 1 , with figure 1 The embodiment of the application provided for the embodiment of the application provides a method for the preparation of an intermediate of fenpyramid, comprising the following steps:

[0035] Generate propionic acid sodium salt by reaction of liquid caustic soda and (R)-(+)-2-(4-hydroxyphenoxy) propionic acid (hereinafter referred to as propionic acid), the reaction formula is as follows:

[0036]

[0037] Add toluene to the propionate sodium salt adjusted to a certain pH value, replace the solvent for dehydration under low temperature and negative pressure, and end the dehydration when the water content in the system is less than 0.1%;

[0038] After the dehydration is completed, add 2,6-dichlorobenzoxazolone and mix evenly to obtain a mixed system;

[0039] Add salt of wormwood and catalyzer tetrabutyl ammonium bromide to mixing system by the mode of a small amount many times;

[0040] After the reaction is...

example 1

[0044] 1. Add 246.8g of 25% liquid caustic soda into a 1000ml four-neck flask and start stirring.

[0045] 2. Weigh 132.2g of propionic acid and add it to the liquid caustic soda several times in small amounts. The control time is 1 hour. After the dropwise addition, keep warm at 40-50°C for two hours, then take a sample and analyze that the propionic acid content is less than 0.1%. If the reaction is qualified, proceed to the next step.

[0046] 3. After adjusting the pH to 12 with 10% hydrochloric acid, add 400ml of toluene frame negative pressure oil-water separation device to dehydrate until the water content is less than 0.05%.

[0047] 4. After cooling down to room temperature, add 140.2 g of molten dichloride into the flask and stir evenly.

[0048] 5. Add 77.2g of potassium carbonate and 6g of tetrabutylammonium bromide through the feeding funnel for 1 hour.

[0049] 6. Raise the temperature to 80° C. and keep it warm for 8 hours to react. Sampling and analyzing the r...

example 2

[0055] 1. Add 246.5g of 25% liquid caustic soda into a 1000ml four-neck flask and start stirring.

[0056] 2. Weigh 132.4g of propionic acid and add it to the liquid caustic soda in small amounts for several times. The control time is 1 hour. After the dropwise addition, keep warm at 40-45°C for two hours, then take a sample and analyze that the propionic acid content is less than 0.1%. If the reaction is qualified, proceed to the next step.

[0057] 3. After adjusting the pH to 12 with 10% hydrochloric acid, add 400ml of toluene frame negative pressure oil-water separation device to dehydrate to 0.07% moisture.

[0058] 4. After cooling down to room temperature, add 140.3 g of molten dichloride into the flask and stir evenly.

[0059] 5. Add 77.0g of potassium carbonate and 6g of tetrabutylammonium bromide through the feeding funnel for 1 hour.

[0060] 6. Raise the temperature to 80° C. and keep it warm for 8 hours to react. Sampling and analyzing the residue of dichloride ...

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Abstract

The invention provides an metamifop intermediate and a preparation method of metamifop. The preparation method comprises the following steps: reacting caustic soda liquid with (R)-(+)-2-(4-hydroxyphenoxy) propionic acid to generate sodium propionate; adding toluene into the sodium propionate after the pH value is adjusted to a certain value, carrying out solvent replacement dehydration in a low-temperature negative-pressure state, and stopping dehydration when the water content in the system is smaller than 0.1%; after dehydration is finished, adding 2, 6-dichlorobenzoxazolone, and uniformly mixing to obtain a mixed system; adding potassium carbonate and catalyst tetrabutylammonium bromide into the mixed system; after the reaction is completed, cooling the system to room temperature, adding a certain amount of water, layering, enabling upper-layer toluene to enter a toluene recovery system, and enabling a lower-layer water phase as an acidification raw material to enter an acidification system; and separating out the material from the water phase by dropwise adding hydrochloric acid, adjusting the pH value of the water phase to be 1-2, centrifuging the material, and drying to obtain condensation compound hydroxyphenoxy propionic acid.

Description

technical field [0001] The present application relates to the technical field of preparation of fenpyramid herbicides, in particular to a preparation method of fenpyralid intermediate and fenpyralid. Background technique [0002] Metamifop (Metamifop) is an aryloxyphenoxypropionate herbicide developed by Korea Chemical Technology Research Institute, which can control most annual grass weeds very well, unlike most of these herbicides Yes, fenpyramid is safe for rice, and can effectively control the main weeds in rice fields, such as barnyardgrass, stephenia, crabgrass and goosegrass, and is mainly used for weeding in transplanted and direct seeded rice fields. Mefenpyramid has low toxicity, is environmentally safe, has wide compatibility, and is expected to be used for weeding other crops and lawns. It is a promising herbicide. Methafen is a new type, high efficiency, low toxicity, environment-friendly aryloxyphenoxypropionate herbicide, which belongs to aryloxyphenoxypropio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D263/58
CPCC07D263/58
Inventor 王龙张海松郭超王林梁院龙赵乐
Owner 宁夏蓝田农业开发有限公司
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