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Method for preparing ethylsulfonyl acetonitrile

A technology of ethylsulfonylacetonitrile and ethylthioacetonitrile, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problem of high price of oxidant m-chloroperoxybenzoic acid, and achieve mild reaction and high content The effect of high and low dosage

Inactive Publication Date: 2008-01-09
HUNAN CHEM RES INST
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AI Technical Summary

Problems solved by technology

[0006] In these existing methods, method 1. the price of oxidant m-chloroperoxybenzoic acid used is expensive

Method used

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  • Method for preparing ethylsulfonyl acetonitrile
  • Method for preparing ethylsulfonyl acetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 375.0g (3.71mol) of ethylthioacetonitrile, 225.0g (3.75mol) of acetic acid and 18.0g of tungsten dihydrate to a 3000mL three-necked flask equipped with a thermometer, condenser, constant pressure dropping funnel, and stirrer Sodium acid, add 984.0g (7.8mol) hydrogen peroxide (content 27.0%) dropwise at room temperature, stir and react at 40°C to 50°C for 2 hours, then distill off about 750.0g aqueous acetic acid solution under reduced pressure. Cool and add enough water to dissolve the salt. The oil layer was separated, and the water layer was extracted twice with 500 mL of chloroform. The organic layers were combined, and the chloroform was recovered under reduced pressure to obtain 461.9 g of the product, with a crude yield of 93.6% and a content of 98.4% (quantitative analysis by gas chromatography). 1 H NMR (CDCl 3 )δ: (ppm) 1.50 ~ 1.55 (t, 3H, -CH 2 C H 3 ), 3.30~3.37 (q, 2H, -CH 2 -), 3.97~3.98(m, 2H, -CH 2 CN).

Embodiment 2

[0015] Add 375.0g (3.71mol) of ethylthioacetonitrile, 225.0g (3.75mol) of acetic acid and 18.0g of tungsten dihydrate to a 3000mL three-necked flask equipped with a thermometer, condenser, constant pressure dropping funnel, and stirrer Sodium acid, add 984.0g (7.8mol) hydrogen peroxide (content 27.0%) dropwise at room temperature, stir and react at 40°C to 50°C for 2 hours, then distill off about 750.0g aqueous acetic acid solution under reduced pressure. Cool and add enough water to dissolve the salt. The oil layer was separated, and the aqueous layer was extracted twice with 500 mL of ethyl acetate. The organic layers were combined, and ethyl acetate was recovered under reduced pressure to obtain 470.0 g of the product, with a crude yield of 95.2% and a content of 98.6% (quantitative analysis by gas chromatography).

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Abstract

Preparation of ethylsulfonyl-methyl cyanide is carried out by: taking acetic acid as reactive solvent, taking hydrogen peroxide as oxidant and oxidizing ethyl phenyl methyl cyanide into ethylsulfonyl-methyl cyanide. It's convenient, controllable and efficient. It has gentle reactive condition, higher content and can be used for industrial production. It can be used to produce super-efficient sulfonylurea herbicide jade pyrsulfogentian intermediate.

Description

technical field [0001] The present invention relates to the preparation method of ethanesulfonyl acetonitrile. Background technique [0002] Ethylacetonitrile is an intermediate for preparing the super-efficient sulfonylurea herbicide rimsulfuron-methyl (patent US4774337). According to bibliographical reports, ethylsulfonyl acetonitrile is prepared by oxidizing thioether compound ethylthio acetonitrile into sulfone, and the method mainly contains the following: [0003] ①. Using dichloromethane as solvent and m-chloroperoxybenzoic acid as oxidant (WO Patent 2004101505). [0004] ②. Use acetic acid as solvent and sodium perborate hydrate as oxidant (Nie Hui, Tong Xiaoxu, Wu Ciwen. Hebei Chemical Industry. 1996, 4: 38-45. Zhou Weiqing, Zhang Likang, Xu Xiaoqing, Zhang Zheng. Journal of Inorganic Chemistry. 1992, 1( 8): 88~90. Yue Guoren, Wang Jianhua, Zhang Zheng. Applied Chemistry. 1995, 12(4): 93~95. etc.). [0005] ③. Using acetic acid as solvent and hydrogen peroxide as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/26C07C315/02
Inventor 毛春晖冯现同陈明黄明智杨彬
Owner HUNAN CHEM RES INST
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