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Synthetic method for organically compounding intermediate cyanogen

A technology for the synthesis of ethanedinitrile and a synthetic method, which is applied in the field of synthesis of the organic synthesis intermediate ethanedinitrile, can solve the problems of low final yield and complicated process, shorten the reaction time, reduce intermediate links, and improve the reaction rate. Yield effect

Inactive Publication Date: 2018-07-10
CHENGDU DONG DIAN AI ER TECH
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Problems solved by technology

However, most of the existing synthetic methods use sodium cyanide as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which is helpful for further improving the quality and yield of the product. , it is of great economic significance to reduce the content of by-products

Method used

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  • Synthetic method for organically compounding intermediate cyanogen

Examples

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example 1

[0011] Dissolve 5mol of 1,4-diiodobutane in 5L of 30% acetone solution, control the stirring speed at 110rpm, add 6mol of 4-methyl-benzonitrile, raise the temperature of the solution to 60℃, and reflux for 90min , Reduce the temperature of the solution to 10℃, filter, wash the filter cake with 50% methylamine solution with mass fraction, pour into 20% potassium iodide solution with mass fraction, and the oil layer should be washed with sodium chloride solution, mass fraction is 70% Washing with pentane solution, washing with 80% ethyl acetate solution with mass fraction, 30kPa vacuum distillation, collecting 50°C fractions, dehydrating with anhydrous sodium sulfate dehydrating agent, to obtain 480.6g of finished oxonitrile with a yield of 89%.

example 2

[0013] Dissolve 5mol of 1,4-diiodobutane in 5L of 32% acetone solution, control the stirring speed to 130rpm, add 6.5mol of 4-methyl-benzonitrile, raise the temperature of the solution to 65℃, and reflux 100min, reduce the temperature of the solution to 12℃, filter, wash the filter cake with a mass fraction of 52% methylamine solution, pour into a 23% potassium iodide solution, and then layer the oil layer with sodium chloride solution, the mass fraction is 72 Wash with %pentane solution, wash with 82% ethyl acetate solution, 35kPa vacuum distillation, collect the 52°C distillate, and dehydrate with anhydrous potassium carbonate dehydrating agent to obtain 491.4g of finished oxonitrile with a yield of 91%.

example 3

[0015] Dissolve 5mol of 1,4-diiodobutane in 5L of 35% acetone solution, control the stirring speed at 150rpm, add 7mol of 4-methyl-benzonitrile, raise the temperature of the solution to 70℃, and reflux for 110min , Reduce the temperature of the solution to 15℃, filter, wash the filter cake with a 55% mass fraction of methylamine solution, pour into a 27% mass fraction of potassium iodide solution, layering occurs, and wash the oil layer with sodium chloride solution, with a mass fraction of 75% Washing with pentane solution, washing with 85% ethyl acetate solution with mass fraction, 40kPa vacuum distillation, collecting 55°C distillate, dehydrating with anhydrous sodium sulfate dehydrating agent, to obtain 507.6g of finished oxonitrile with a yield of 94%.

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Abstract

Provided is a synthetic method for organically compounding intermediate cyanogen. The method mainly comprises the following steps that 5 moles of 1,4-diiodobutane dissolves in 5 liters of acetone solution, the stirring speed is controlled at 110-150 revolutions per minute, 6-7 moles of 4-methyl-benzonitrile is added into, the temperature of the solution is heated to 60-70 DEG C, circulation refluxis carried out for 90-110 minutes, the temperature of the solution is reduced to 10-15 DEG C, filtering is carried out, a filter mass is washed by a methylamine solution, and then poured into a potassium iodide solution, stratification occurs, an oil layer is washed by a sodium chloride solution, pentane solution and ethyl acetate solution in sequence, reduced pressure distillation is carried out, cut fraction of 50-55 DEG C is collected, dehydration is carried out by using a dehydrating agent, and finished cyanogen is obtained.

Description

Technical field [0001] The invention relates to a method for synthesizing oxonitrile, an intermediate in organic synthesis. Background technique [0002] Oxalonitrile is mainly used to manufacture nylon intermediates. However, most of the existing synthesis methods use sodium cyanide as the reactant, the process is relatively complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthesis method, which is useful for further improving the quality and yield of the product. , Reducing the content of by-products has important economic significance. Summary of the invention [0003] The purpose of the present invention is to provide a method for synthesizing oxonitrile, an intermediate in organic synthesis, which includes the following steps: [0004] (i) Dissolve 5mol of 1,4-diiodobutane in 5L of acetone solution, control the stirring speed at 110-150rpm, add 6-7mol of 4-methyl-benzonitrile, and raise the solution temperature to 60-70 ℃, reflu...

Claims

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Application Information

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IPC IPC(8): C07C255/04C07C253/00
CPCC07C253/00C07C255/04
Inventor 严义达
Owner CHENGDU DONG DIAN AI ER TECH
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