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Preparation method of 2,3-bis(benzylamino)butanedioic acid

A technology based on succinic acid and benzylamino, which is applied in the field of preparation of 2,3-bis(benzylamino)succinic acid, can solve problems such as low recovery rate, low yield, and dark product appearance, and achieve Reduced overall cost, reduced benzylamine dosage, and whiter appearance

Inactive Publication Date: 2015-11-18
ANHUI LANGXI LIANKE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method is very difficult to control. It is a heating reaction itself, and it will release heat when the reaction is triggered. Once the control is not good, it will be dangerous. At the same time, the holding time is very long, the yield is low, and the high cost of more than three times the theoretical amount is required. benzylamine, the recovery rate is not high and the energy consumption is large, and the obtained product appearance color is very dark, it is difficult to decolorize

Method used

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Embodiment 1

[0018] A kind of preparation method of 2,3-two (benzylamino) succinic acid, comprises the steps:

[0019] In the first step, get 2,3-dibromosuccinic acid and put it into the reaction kettle, add ethanol and stir and dissolve to obtain 2,3-dibromosuccinic acid ethanol solution;

[0020] Second step, add the concentrated sulfuric acid that mass concentration is 98% to carry out esterification;

[0021] In the third step, benzylamine is added dropwise, and the dropwise addition is completed and the temperature is raised to reflux for 4 hours;

[0022] The 4th step, rectification reclaims ethanol;

[0023] The fifth step is to lower the temperature and adjust the acid to hydrolyze;

[0024] The sixth step is centrifugation to obtain white 2,3-bis(benzylamino)succinic acid solid.

[0025] The molar ratio of 2,3-dibromosuccinic acid to ethanol is 1:3.8.

[0026] The molar ratio of the 2,3-dibromosuccinic acid to the benzylamine is 1:1.2.

[0027] The preparation method of the p...

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Abstract

The invention discloses a preparation method of 2,3-bis(benzylamino)butanedioic acid. The method comprises the following steps: 1, adding 2,3-dibromobutanedioic acid into a reaction kettle, adding ethanol, and stirring for dissolving to obtain an ethanol solution of 2,3-dibromobutanedioic acid; 2, adding concentrated sulfuric acid with the mass concentration of 98%, and carrying out an esterification reaction; 3, adding benzylamine in a dropwise manner, and carrying out heating refluxing for 4h after the dropwise addition ends; 4, rectifying to recover ethanol; 5, cooling, and carrying out acid regulation hydrolysis; and 6, centrifuging, and separating to obtain white 2,3-bis(benzylamino)butanedioic acid solid. A carboxyl group is protected in the preparation method of 2,3-bis(benzylamino)butanedioic acid in order to reduce the use amount of benzylamine, so the comprehensive cost decreases by 10% or above, the yield increases by 5%, the obtained product has white appearance, and the method is suitable for industrial large-scale production.

Description

technical field [0001] The invention specifically relates to a preparation method of 2,3-bis(benzylamino)succinic acid, belonging to the field of chemical industry. Background technique [0002] 2,3-bis(benzylamino)succinic acid is an essential intermediate for the synthesis of vitamin H, and is also widely used in chemical organic synthesis. Existing preparation 2, the method for two (benzylamino) succinic acid of 3-bis (benzylamino) succinic acid is: benzyl amine is dripped in 2, in the 3-dibromosuccinic acid ethanol solution, when benzyl amine reaches suitable concentration, reaction begins to be Initiation, after 12 hours of heat preservation reaction, the product is gradually precipitated in ethanol, and the product is obtained by centrifugation after recovering ethanol. But this method is very difficult to control. It is a heating reaction itself, and it will release heat when the reaction is triggered. Once the control is not good, it will be dangerous. At the same t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/26C07C227/04
Inventor 贾玉梁张富成
Owner ANHUI LANGXI LIANKE IND
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