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A kind of preparation method of furansulcotrione

A technology of furansulcotrione and tetrahydrofuran, which is applied in the field of compound synthesis, can solve the problems of lowering furansulcotrione yield, complex reaction steps, complicated preparation process, etc., and achieves environmental protection, less reaction process, and simple preparation process Effect

Active Publication Date: 2020-12-29
安徽工大化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The traditional preparation process of furansulcotrione is to form ether at last, because the yield of ether-forming reaction is relatively low, resulting in low yield in the traditional preparation method of furansulcotrione, and the preparation process is more complicated, involving multi-step reactions, The complexity of the reaction steps has led to an increase in side reactions, thereby reducing the yield of furansulcotrione

Method used

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  • A kind of preparation method of furansulcotrione
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  • A kind of preparation method of furansulcotrione

Examples

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Effect test

Embodiment 1

[0035] Take 20ml of methanol into a three-neck bottle, then weigh 3g of 2-chloro-3-methyl-4-methanesulfonylbenzoic acid and add it, then put it into the rotor, add 10ml of methanol, install a reflux device and a thermometer, and The mouth is coated with vacuum ester, so that the whole reaction is carried out in a sealed environment. Move the device to a magnetic stirrer and start stirring, then slowly add 1.35 g of thionyl chloride dropwise in batches. After the addition, heat up and control the temperature at 60°C. After stirring for 3 hours, the reaction is complete, and the solution turns into an oily clear liquid. Stop stirring and stop heating. Take a 350ml beaker and add tap water, the amount added is half of the capacity of the beaker, after the reaction solution is naturally cooled, pour the reaction solution into the beaker, the reaction solution quickly crystallizes into a white solid, then suck the solid by suction filtration, put the solid in an oven to dry , to o...

Embodiment 2

[0040] Take 20ml of methanol into a three-neck bottle, then weigh 3g of 2-chloro-3-methyl-4-methanesulfonylbenzoic acid and add it, then put it into the rotor, add 10ml of methanol, install a reflux device and a thermometer, and The mouth is coated with vacuum ester, so that the whole reaction is carried out in a sealed environment. Move the device to a magnetic stirrer and start stirring, then slowly add concentrated sulfuric acid dropwise in 3 times. The total amount of concentrated sulfuric acid added is 1.35g. After the addition, heat up and control the temperature at 62.5°C. After stirring for 7 hours, the reaction is complete. , the solution completely turns into an oily clear liquid, stop stirring and stop heating. Take a 350ml beaker and add tap water, the amount added is half of the capacity of the beaker. After the reaction solution cools down naturally, pour the reaction solution into the beaker. The reaction solution quickly crystallizes into a white solid, then su...

Embodiment 3

[0045] Take 20ml of methanol into a three-neck bottle, then weigh 3g of 2-chloro-3-methyl-4-methanesulfonylbenzoic acid and pour it into the bottle, then put it into the rotor, add 10ml of methanol, and install a reflux device and a thermometer , the bottle mouth is coated with vacuum ester so that the whole reaction is carried out in a sealed environment. Move the device to a magnetic stirrer and start stirring, then slowly add 1.35 g of concentrated sulfuric acid dropwise in 3 batches. After the addition, heat up and control the temperature at 65°C. After stirring for 7 hours, the reaction is complete, and the solution turns into an oily clear liquid. Stop stirring and stop heating. Take a 350ml beaker and add tap water, the amount added is half of the capacity of the beaker, after the reaction solution is naturally cooled, pour the reaction solution into the beaker, the reaction solution quickly crystallizes into a white solid, then suck the solid by suction filtration, put...

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Abstract

The invention provides a preparation method for tefuryltrione, and belongs to the technical field of compound preparation. The preparation method comprises the following steps that esterification reaction is carried out on 2-chloro-3-methyl-4-methylsulfonylbenzoic acid serving as a raw material and methanol so as to generate methyl 2-chloro-3-methyl-4- methanesulfonylbenzoate; then reaction is carried out with N-bromosuccinimide to replace one hydrogen in a methyl group on a benzene ring so as to generate methyl 2-chloro-3-methyl bromide-4-methanesulfonylbenzoate; then a product of methyl 2-chloro-4-(methylsulfonyl)-3-(((tetrahydrofuran-2-yl)methoxy)methyl) benzoate is synthesized by using a Williamson synthesis method; and then condensation reaction is carried out with cyclohexanedione under the action of ethylene diamine so as to generate enol ester, and finally, acetonitrile is added for rearrangement catalysis under the action of the ethylene diamine so as to obtain a target product of the tefuryltrione. The preparation method has the advantages of being mild in reaction conditions and simple in synthesis steps.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a preparation method of furansulcotrione. Background technique [0002] In recent years, the country implements preferential policies for subsidizing early rice planting, which makes the domestic early rice planting area increase year by year. At the same time, due to the vigorous promotion of the crop rotation model, the proportion of the direct-seeding rice cultivation area has continued to expand, but the problem of weed damage caused by it is also more prominent. Weeding is often caused by untimely weeding or inadequate technology. At the same time, long-term use of single or Similar herbicide varieties increase the resistance of weeds, which in turn leads to the decline of rice quality, yield loss, and even grain failure. As a new type of high-efficiency herbicide, furasulcotrione has become a research and development hotspot. [0003] Furosulcotrione, the struc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/12
CPCC07D307/12
Inventor 宋丰发张仲谋许立信万超
Owner 安徽工大化工科技有限公司
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