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Synthesis method of ethyl N-cyanoethanimideate

A technology of ethyl cyanoethylimidate and ethyl ethylimidate hydrochloride, applied in the direction of organic chemistry, etc., can solve production costs, high energy consumption, difficult to handle by-products, low yield, low purity, etc. problem, to achieve the effect of increasing the content, avoiding inseparability, and simple process steps

Inactive Publication Date: 2019-09-20
宁夏贝利特生物科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In view of this, the object of the present invention is to overcome the problems of high production cost, high energy consumption, low yield and purity, and difficult to handle by-products in the prior art, and provide a high-yield, low-energy-consumption, single by-product A kind of synthetic method of ethyl N-cyanoethylimidate

Method used

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  • Synthesis method of ethyl N-cyanoethanimideate
  • Synthesis method of ethyl N-cyanoethanimideate
  • Synthesis method of ethyl N-cyanoethanimideate

Examples

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Embodiment 1

[0038] Add 505.1 g of ethyl imidate hydrochloride in a stirred reactor, add 544.0 g of cyanamide aqueous solution with a mass concentration of 30% under stirring, stir for 3 minutes to make ethyl imidate hydrochloride After the acid salt is fully dissolved, start to add dropwise a mass percent concentration of 30% sodium hydroxide aqueous solution, adjust the pH value of the solution in the reactor to about 6.5, and after reacting for 60 minutes at normal temperature, get the organic phase for gas chromatography analysis. The ester content is: 97.2%.

[0039] After the reaction, the system is poured into a separatory funnel at room temperature to allow it to be layered. The lower layer is an aqueous phase, and the upper layer is an organic phase. The organic phase can be distilled under reduced pressure to obtain high-purity ethyl N-cyanoethylimidate. Ester product, the content of cyanoethyl ester in the final product is: 99.8%, total yield: 83%; After the water phase remainin...

Embodiment 2

[0041] Add 505.1 g of ethyl acetimidate hydrochloride in a stirred reactor, add 524.1 g of cyanamide aqueous solution with a mass concentration of 25% under stirring, stir for 3 minutes to make ethyl acetimidate hydrochloride After the acid salt is fully dissolved, start to add dropwise a mass percent concentration of 10% sodium hydroxide aqueous solution, adjust the pH value of the solution in the reactor to about 5, and react at normal temperature for 10 minutes, get the organic phase for gas chromatography analysis, and the cyanoethyl The ester content is: 86.9%.

[0042] After the reaction, the system is poured into a separatory funnel at room temperature to allow it to be layered. The lower layer is an aqueous phase, and the upper layer is an organic phase. The organic phase can be distilled under reduced pressure to obtain high-purity ethyl N-cyanoethylimidate. Ester product, the content of cyanoethyl ester in the final product is: 99.6%, total yield: 72%; After the wate...

Embodiment 3

[0044] Add 505.1 g of ethyl imidate hydrochloride in a stirred reactor, add 468.2 g of cyanamide aqueous solution with a mass concentration of 35% under stirring, stir for 3 minutes to make ethyl imidate hydrochloride After the acid salt is fully dissolved, start to add dropwise a mass percent concentration of 20% sodium hydroxide aqueous solution, adjust the pH value of the solution in the reaction kettle to about 6, and after reacting for 30 minutes at normal temperature, get the organic phase for gas chromatography analysis. The ester content is: 93.6%.

[0045] After the reaction, the system is poured into a separatory funnel at room temperature to allow it to be layered. The lower layer is an aqueous phase, and the upper layer is an organic phase. The organic phase can be distilled under reduced pressure to obtain high-purity ethyl N-cyanoethylimidate. Ester product, the content of cyanoethyl ester in the final product is: 99.4%, total yield: 78%; After the water phase re...

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Abstract

The invention discloses a synthesis method of ethyl N-cyanoethanimideate, and the method comprises the following steps: adding ethyl ethyleneimine hydrochloride into a reaction kettle with stirring, adding a cyanamide aqueous solution under stirring, and stirring until the ethyl ethyleneimine hydrochloride is fully dissolved; dropping an alkaline substance to adjust pH value; allowing the materials to be fully reacted under normal temperature and stirring state, taking samples every 10 min in the reaction process, and detecting the samples by chromatography to determine the conversion rate of the reaction; standing after an aqueous phase and an organic phase in the reactant are layered, extracting the organic phase out and then distilling organic phase the under reduced pressure to obtain an ethyl N-cyanoethanimideate product. The synthesis method is simple and feasible, energy-saving and environment-friendly, solves the problems of complex reaction, pollution and the like in the synthesis process, and saves the cost at the same time.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and more specifically relates to a synthetic method of ethyl N-cyanoethylimidate. Background technique [0002] Ethyl cyanoate, also known as ethyl cyanoethylimidate, is an important pharmaceutical and pesticide intermediate for the synthesis of insecticides acetamiprid and vitamin B1, as well as an important chemical raw material. [0003] Many documents in China have described the synthesis of cyanoethyl ester, and the reaction equation of the currently mainly used synthetic cyanoethyl ester is as follows: [0004] [0005] The reaction process mainly has the following problems: [0006] 1. Due to the higher price of the raw material disodium hydrogen phosphate, the production cost is higher; [0007] 2. The generated by-products contain a large amount of sodium dihydrogen phosphate, sodium chloride, and ammonium chloride. This part of the mixed salt is listed in the list of haza...

Claims

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Application Information

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IPC IPC(8): C07C261/04
CPCC07C261/04
Inventor 王辉赵黎明王中杰姬越城苏炜夏学鹏王鑫彤
Owner 宁夏贝利特生物科技有限公司
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