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Synthetic process of dinotefuran

A synthesis process, the technology of dinotefuran, which is applied in the field of pesticide preparation, can solve the problems of high cost, long synthesis time of dinotefuran, and complicated synthesis process, and achieve the effects of low cost, improved environmental protection effect, and simple synthesis process

Inactive Publication Date: 2017-12-22
上海开荣化工科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to solve the problems existing in the above-mentioned prior art, and provides a synthesis process of dinotefuran, which solves the problems of long synthesis time, complicated synthesis process and high cost of dinotefuran, and satisfies the synthesis demand of dinotefuran

Method used

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  • Synthetic process of dinotefuran

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Experimental program
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Effect test

Embodiment 1

[0013] The synthetic technique of this dinotefuran comprises the steps:

[0014] The first step, raw material selection, selects 1,4-butyrolactone as the synthetic raw material for preparing dinotefuran;

[0015] In the second step, the preparation of the intermediate, add 15g of 1,4-butyrolactone, 12g of tribromomethane, 30mL of hydrazine hydrate, and 7g of potassium carbonate in a four-necked reaction flask with a stirrer, a thermometer, and a reflux condenser, and heat Reaction at 70°C for 6 hours. After the reaction is completed, use 12g of diethyl ether to elute. After recovering the diethyl ether, the intermediate 3-(bromomethyl)tetrahydrofuran is obtained, and then add 15g of 3-(bromomethyl)tetrahydrofuran, 12g of lithium hexamethyldisilazide, 6g of potassium carbonate, 6g of sodium sulfate, and 30mL of ethanol were heated to 60°C for 7 hours, and eluted with 12g of diethyl ether after the reaction was completed. After recovering ether, the intermediate 1-(tetrahydro-3...

Embodiment 2

[0018] The synthetic technique of this dinotefuran comprises the steps:

[0019] The first step, raw material selection, selects 1,4-butyrolactone as the synthetic raw material for preparing dinotefuran;

[0020] In the second step, the preparation of the intermediate, add 20g of 1,4-butyrolactone, 13g of tribromomethane, 30mL of hydrazine hydrate, and 8g of potassium carbonate in a four-necked reaction flask with a stirrer, a thermometer, and a reflux condenser, and heat Reaction at 70°C for 7 hours. After the reaction is completed, use 15g of diethyl ether to elute. After recovering the diethyl ether, the intermediate 3-(bromomethyl)tetrahydrofuran is obtained, and then add 20g of 3-(bromomethyl)tetrahydrofuran, 15g of lithium hexamethyldisilazide, 7g of potassium carbonate, 7g of sodium sulfate, and 30mL of ethanol were heated to 60°C for 7 hours, and eluted with 15g of diethyl ether after the reaction was completed. After recovering ether, the intermediate 1-(tetrahydro-3...

Embodiment 3

[0023] The synthetic technique of this dinotefuran comprises the steps:

[0024] The first step, raw material selection, selects 1,4-butyrolactone as the synthetic raw material for preparing dinotefuran;

[0025] In the second step, the preparation of the intermediate, add 30g of 1,4-butyrolactone, 15g of tribromomethane, 30mL of hydrazine hydrate, and 9g of potassium carbonate in a four-necked reaction flask with a stirrer, a thermometer, and a reflux condenser, and heat React at 70°C for 9 hours. After the reaction is completed, use 17g of diethyl ether to elute. After recovering the diethyl ether, the intermediate 3-(bromomethyl)tetrahydrofuran is obtained, and then add 30g of 3-(bromomethyl)tetrahydrofuran, 18g of lithium hexamethyldisilazide, 8g of potassium carbonate, 8g of sodium sulfate, and 30mL of ethanol were heated to 60°C for 7 hours, and eluted with 17g of diethyl ether after the reaction was completed. After recovering ether, the intermediate 1-(tetrahydro-3-fu...

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Abstract

The invention relates to a synthetic process of dinotefuran. The dinotefuran is prepared by raw material selection, intermediate preparation and dinotefuran synthesis. The synthetic process provided by the invention has the benefits that in the preparation process of an intermediate, the dinotefuran can be synthesized only through preparing the intermediate twice; the synthesis process is simple, and the synthesis procedure is simple, so that the whole synthesis procedure of the dinotefuran is simplified, and the synthesis time of the dinotefuran is shortened; in the scale production, the production efficiency is improved, and the production output is improved; the synthesis yield of the dinotefuran is high, and the product yield is high, so that the production cost can be reduced; the use of methanol is eliminated in the synthetic process, so that the generation of pollutants is reduced, safety and environmental protection are realized, and the environmental protection effect is improved; and the use effect is good, and the popularization is facilitated.

Description

technical field [0001] The invention relates to the technical field of pesticide preparation, in particular to a synthesis process of dinotefuran. Background technique [0002] At present, the synthesis process of dinotefuran in the domestic market is complicated, the process is cumbersome, the reaction time is long, and the yield of the target compound is low, resulting in long production time in actual production, low production efficiency, high cost, and waste generated during the synthesis process. More, more pollution, and the actual effect of large-scale production is poor. Contents of the invention [0003] The present invention aims to solve the problems existing in the above-mentioned prior art, and provides a synthesis process of dinotefuran, which solves the current problems of long synthesis time, complicated synthesis process and high cost of dinotefuran, and satisfies the synthesis demand of dinotefuran. [0004] The present invention solves the technical sc...

Claims

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Application Information

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IPC IPC(8): C07D307/14
CPCC07D307/14
Inventor 朱建永刘如成
Owner 上海开荣化工科技有限公司
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