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A method for synthesizing 2-acetoxy-3-butenenitrile

A technology of acetoxy and acrylonitrile, applied in the field of fine chemistry, can solve problems such as unfavorable reactions, processing requirements and high costs, and achieve the effects of reducing costs, improving efficiency, and environmental protection costs

Active Publication Date: 2020-09-18
NANJING REDSUN BIOCHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sodium cyanide aqueous solution forms cyanide-containing wastewater, which has relatively high treatment requirements and costs. At the same time, the cyanide in the sodium cyanide aqueous solution is easy to self-polymerize, which is not conducive to the reaction.

Method used

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  • A method for synthesizing 2-acetoxy-3-butenenitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1 mol of hydrocyanic acid (27g) and 3 mol of methanol (96g) were mixed, and after mixing, the temperature was lowered to -10°C for later use. 1 mol (56 g) of acrolein and 1.01 mol (103.2 g) of acetic anhydride were mixed in a flask equipped with magnetic stirring, and the temperature was lowered to -15°C. Add the mixed solution of acrolein and acetic anhydride to the methanol solution of hydrocyanic acid dropwise for 2 hours. During the dropwise addition, keep the temperature of the flask at -10~-12°C. Finally, a rectification column with 3 trays is used, the substrate is heated, the top reflux ratio is 1:4, and methanol is obtained at 67°C, and acetic acid is obtained at 118°C. After methanol and acetic acid are extracted, the temperature at the bottom of the tower will increase , continue heating, and extract 125.4 g of 2-acetoxy-3-butenenitrile product at 170° C., the purity is 98.5%, and the yield reaches 98.8%.

Embodiment 2

[0024] 1.05 mol of hydrocyanic acid (28.35 g) and 3.15 mol of methanol (100.8 g) were mixed, and after mixing, the temperature was lowered to -10°C for later use. 1 mol (56 g) of acrolein and 1.2 mol (122.4 g) of acetic anhydride were mixed in a flask equipped with magnetic stirring, and the temperature was lowered to -15°C. Add the mixed solution of acrolein and acetic anhydride to the methanol solution of hydrocyanic acid dropwise for 2 hours. During the dropwise addition, keep the temperature of the flask at -10~-12°C. Finally, referring to the rectification conditions in Example 1, 125.5 g of 2-acetoxy-3-butenenitrile product was obtained with a purity of 98.8% and a yield of 99.2%.

Embodiment 3

[0026] 1 mol of hydrocyanic acid (27g) and 3 mol of methanol (96g) were mixed, and after mixing, the temperature was lowered to -10°C for later use. 1 mol (56 g) of acrolein and 1.01 mol (103.2 g) of acetic anhydride were mixed in a flask equipped with magnetic stirring, and the temperature was lowered to -5°C. Add the mixed solution of acrolein and acetic anhydride to the methanol solution of hydrocyanic acid dropwise for 2 hours. During the dropwise addition, keep the temperature of the flask at -2~0°C. After the dropwise addition, continue the heat preservation reaction for 1 hour. , with reference to the rectifying conditions of Example 1, 116.2 g of 2-acetoxy-3-butenenitrile product was obtained, the purity was 92.5%, and the yield reached 86%.

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Abstract

The invention discloses a method for synthesizing 2-acetoxyl-3-crotononitrile. The method comprises the following steps: taking acrolein, hydrocyanic acid and acetic anhydride as raw materials, dropping mixed solution of the acrolein and the acetic anhydride into alcoholic solution of the hydrocyanic acid, performing a reaction on the mixture, so as to obtain the 2-acetoxyl-3-crotononitrile. In the method, the hydrocyanic acid replaces sodium cyanide which is used for performing a reaction with water, so that the problem that cyanide-containing waste water caused by the use of the water in thesynthesis process is avoided, and the 2-acetoxyl-3-crotononitrile is efficiently synthesized. In the method, alcohol is taken as a reaction system, acetic acid is generated in the reaction process, and all solvents can be recycled, therefore, the method has the advantages of being environmentally friendly and lowering the cost.

Description

technical field [0001] The invention belongs to the field of fine chemistry, and in particular relates to a method for synthesizing a pesticide intermediate 2-acetoxy-3-butenenitrile. Background technique [0002] 2-Acetoxy-3-butenenitrile (ACA) was first proposed by Hoechst (Bayer) as an important intermediate in the synthesis of glufosinate-ammonium. Hoechst obtained 2-acetoxy-3-butenenitrile by esterification of acrolein cyanohydrin with acetic anhydride in 1980, and obtained 2-acetoxy-3-butene nitrile with acrolein and sodium cyanide aqueous solution and acetic anhydride in 1982. - Acrylonitrile. Sodium cyanide aqueous solution forms cyanide-containing wastewater, which has relatively high treatment requirements and costs. At the same time, the cyanide in the sodium cyanide aqueous solution is easy to self-polymerize, which is not conducive to the reaction. Contents of the invention [0003] The object of the present invention is to provide a kind of synthesis 2-acet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/15C07C253/00
CPCC07C253/00C07C255/15
Inventor 王述刚岳瑞宽薛谊陈新春杜翔蒋剑华王福军
Owner NANJING REDSUN BIOCHEM CO LTD
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