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Synthesis method for organic synthesis of intermediate adipamide

A technology for the synthesis of adipamide and adipamide, which is applied in the field of synthesis of adipamide as an intermediate in organic synthesis, can solve the problems of low final yield and complicated process, and shorten the reaction time and reduce intermediate link, the effect of improving the reaction yield

Inactive Publication Date: 2018-07-06
CHENGDU DONG DIAN AI ER TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the existing synthetic methods use ammonia 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 will further improve the quality and yield of the product, reduce the By-product content is economically important

Method used

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  • Synthesis method for organic synthesis of intermediate adipamide

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Effect test

example 1

[0011] Add 4 mol of dimethyl adipate, 5 mol of p-toluidine solution, and 6 mol of aqueous solution into the reaction vessel, raise the temperature of the solution to 40°C, control the stirring speed at 110rpm, stir for 50min, let it stand for 90min, and lower the temperature of the solution to 10°C , to precipitate crystals, filter, wash with a mass fraction of 15% potassium bromide solution, wash with a mass fraction of 75% acetonitrile solution, wash with a mass fraction of 85% cyclohexane solution, and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain the finished adipyl Diamine 512.64g, yield 89%.

example 2

[0013] Add 4 mol of dimethyl adipate, 5.5 mol of p-toluidine solution, and 6 mol of aqueous solution in the reaction vessel, raise the solution temperature to 42°C, control the stirring speed at 120rpm, stir for 60min, let it stand for 110min, and lower the solution temperature to 12 ℃, precipitated crystals, filtered, washed with a mass fraction of 17% potassium bromide solution, washed with a mass fraction of 78% acetonitrile solution, washed with a mass fraction of 87% cyclohexane solution, and dehydrated with anhydrous magnesium sulfate dehydrating agent to obtain the finished product Hexadiene Acyl diamide 524.16g, yield 91%.

example 3

[0015] Add 4 mol of dimethyl adipate, 6 mol of p-toluidine solution, and 6 mol of aqueous solution into the reaction vessel, raise the temperature of the solution to 45°C, control the stirring speed at 130rpm, stir for 70min, let it stand for 120min, and lower the solution temperature to 15°C , to precipitate crystals, filter, wash with a mass fraction of 20% potassium bromide solution, wash with a mass fraction of 80% acetonitrile solution, wash with a mass fraction of 90% cyclohexane solution, and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain the finished adipyl Diamine 535.68g, yield 93%.

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Abstract

The invention relates to a synthesis method for organic synthesis of an intermediate adipamide. The method mainly includes the steps of: adding 4mol dimethyl adipate, a 5-6mol p-toluidine solution, and a 6mol aqueous solution into a reaction container, raising the temperature of the solution to 40-45DEG C, controlling the stirring speed at 110-130rpm, performing stirring for 50-70min, conducting standing for 90-120min, lowering the solution temperature to 10-15DEG C, precipitating crystals, conducting filtering, and performing washing with a potassium bromide solution, an acetonitrile solutionand a cyclohexane solution, and conducting dehydration with a dehydrant, thus obtaining the finished product adipamide.

Description

technical field [0001] The invention relates to a method for synthesizing an organic synthesis intermediate adipamide. Background technique [0002] Adipamide is mainly used in intermediate reactions in organic synthesis. However, most of the existing synthetic methods use ammonia 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 will further improve the quality and yield of the product, reduce the The by-product content is of great economic importance. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of organic synthesis intermediate adipamide, comprising the steps: [0004] (i) Add 4mol dimethyl adipate, 5-6mol p-toluidine solution, and 6mol aqueous solution into the reaction vessel, raise the solution temperature to 40-45°C, control the stirring speed at 110-130rpm, and stir for 50-70min , stand still...

Claims

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Application Information

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IPC IPC(8): C07C233/05C07C231/02
CPCC07C231/02C07C233/05
Inventor 严义达
Owner CHENGDU DONG DIAN AI ER TECH
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