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Synthesis technology for spirotetramat

A technology for the synthesis of spirotetramat and its application in the field of pesticides can solve the problems of high by-products and low yields, and achieve the effects of reducing the generation of by-products, increasing the amount of synthesis, and facilitating promotion

Inactive Publication Date: 2017-12-08
上海开荣化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention will solve the problems in the above-mentioned prior art, provide a synthesis process of spirotetramat, solve the problems of low yield and high by-products in the current synthesis process of spirotetramat, and meet the synthesis requirements of spirotetramat

Method used

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  • Synthesis technology for spirotetramat

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The synthesis process of spirotetramat includes the following steps:

[0014] In the first step, raw material selection, cis-8-methoxy-1,3-diazaspiro[4,5]dec-2,4-dione is selected as the raw material for preparing spirotetramat;

[0015] In the second step, the synthesis of intermediates, 10g of cis-8-methoxy-1,3-diazaspiro[4,5]dec-2,4-dione, 2g sodium bicarbonate, 2g silicic acid Put the salt into the reaction tank, then heat to 120°C, react for 26 hours, cool to room temperature after the reaction, adjust the pH to 4, and obtain a brown-red solid. The brown-red solid is cis-4-methoxycyclohexyl-1- Carbamate, then put 10g of cis-4-methoxycyclohexyl-1-carbamic acid and 40mL methanol into the reaction tank, heat up to 50℃ and react for 6h. After the reaction, distill under reduced pressure to obtain a white solid. The white solid is cis-4-methoxycyclohexyl-1-carbamate hydrochloride, followed by 6g of cis-4-methoxycyclohexyl-1-carbamate hydrochloride, 1g potassium carbonate, 2...

Embodiment 2

[0018] The synthesis process of spirotetramat includes the following steps:

[0019] In the first step, raw material selection, cis-8-methoxy-1,3-diazaspiro[4,5]dec-2,4-dione is selected as the raw material for preparing spirotetramat;

[0020] The second step, the synthesis of intermediates, 12g of cis-8-methoxy-1,3-diazaspiro[4,5]dec-2,4-dione, 3g sodium bicarbonate, 3g silicic acid Put the salt into the reaction tank, then heat to 120°C, react for 26 hours, cool to room temperature after the reaction, adjust the pH to 4, and obtain a brown-red solid. The brown-red solid is cis-4-methoxycyclohexyl-1- Carbamate, then 12g of cis-4-methoxycyclohexyl-1-carbamic acid and 40mL methanol were put into the reaction tank, heated to 50°C for 6h, after the reaction, distilled under reduced pressure to obtain a white solid, the white solid was cis-4-methoxycyclohexyl-1-carbamate hydrochloride, followed by 7g of cis-4-methoxycyclohexyl-1-carbamate hydrochloride, 2g potassium carbonate, 20mL a...

Embodiment 3

[0023] The synthesis process of spirotetramat includes the following steps:

[0024] In the first step, raw material selection, cis-8-methoxy-1,3-diazaspiro[4,5]dec-2,4-dione is selected as the raw material for preparing spirotetramat;

[0025] The second step, the synthesis of intermediates, 15g of cis-8-methoxy-1,3-diazaspiro[4,5]dec-2,4-dione, 4g sodium bicarbonate, 5g silicic acid Put the salt into the reaction tank, then heat to 120°C, react for 26h, cool to room temperature after the reaction, adjust the pH to 5, and obtain a brown-red solid, and the brown-red solid is cis-4-methoxycyclohexyl-1- Carbamate, then 15g of cis-4-methoxycyclohexyl-1-carbamic acid and 40mL methanol are put into the reaction tank, heated to 50°C for 6h, after the reaction, it is distilled under reduced pressure to obtain a white solid, the white solid is cis-4-methoxycyclohexyl-1-carbamate hydrochloride, followed by 8g of cis-4-methoxycyclohexyl-1-carbamate hydrochloride, 3g potassium carbonate, 20m...

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Abstract

The invention discloses a synthesis technology for spirotetramat, and is carried out through steps including raw material selection, intermediate synthesis and spirotetramat synthesis. The synthesis technology has the beneficial effects that a synthesis process is simple, byproducts production can be reduced in the synthesis process, byproducts entering next-step reaction can be reduced, the synthesis efficiency of the spirotetramat is improved, the economic benefit of an enterprise is improved, a use effect is good, and the synthesis technology is favorable for popularization.

Description

Technical field [0001] The present invention relates to the technical field of pesticides, in particular to a synthesis process of Spirotetramat. Background technique [0002] Spirotetramat is a novel insecticide and snailicide developed by Bayer, which is a quaternary keto acid compound. It is a lipid synthesis inhibitor that inhibits the synthesis of insect lipids and causes its poisonous death. It is the only insecticide and acaricide with two-way systemic conductivity so far. It has a long-lasting effect and can effectively control various piercing and sucking pests and harmful mites. It can move up and down in the entire plant body and reach the leaf surface. And bark, this unique systemic performance can protect new stems, leaves and roots. Summary of the invention [0003] The present invention aims to solve the above-mentioned problems existing in the prior art, provide a synthesis process of spirotetramat, solve the problems of low yield and high by-products in the curr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/54
Inventor 刘如成朱建永
Owner 上海开荣化工科技有限公司
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