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N-phenylacetyl-L-glutamine

A technology of glutamine and phenylacetyl group, applied in the production field of N-phenylacetyl-L-glutamine, can solve problems such as unfavorable production and use, long synthesis steps, low product purity, etc., and achieves improved production efficiency, The effect of reducing production cost and improving purity

Inactive Publication Date: 2013-08-07
SUZHOU YUANFANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional N-phenylacetyl-L-glutamine synthesis steps are long, the yield is low, generally around 60%, and the product purity is low, so it is not used in subsequent production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Add 200g of tap water and 100g of glutamine into a 1000mL four-necked reaction flask and keep the temperature of the reaction solution lower than 20°C, add 400g of liquid caustic soda with a mass fraction of 15% dropwise, and stir for 10 minutes after the dropwise addition, so that The reaction solution is clarified;

[0017] (2) Control the reaction liquid below 20°C and continue to add 105g of phenylacetyl chloride dropwise. After the dropwise addition, the pH value of the reaction liquid is around 14 and keep it warm at 20°C for 1 hour to ensure the complete reaction of the raw materials;

[0018] (3) After the reaction, control the temperature at 20-25°C, add concentrated hydrochloric acid dropwise and test with a pH meter to make the pH of the solution 7, add 30g of toluene for extraction, control the temperature of the water layer at 40°C and concentrate under reduced pressure to half of the original volume ;

[0019] (4) Cool the concentrated water layer to ...

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PUM

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Abstract

The invention discloses a production method of N-phenylacetyl-L-glutamine, which comprises the following steps: dropwisely adding an alkali solution into a reaction solution of water and glutamine until the reaction solution is clarified, further dropwisely adding phenylacetyl chloride, and then reacting at room temperature for 0.5-2 hours to obtain a mixed solution; and concentrating the mixed solution, regulating the pH value with hydrochloric acid until a crude product is precipitated, and refining with water to obtain the N-phenylacetyl-L-glutamine. In such manner, the invention provides a production method of N-phenylacetyl-L-glutamine. According to the production method, the yield of the obtained product is increased to 80%, the purity is greatly improved, the intermediate control process is changed, the production difficulty for one-step production is reduced, the production efficiency is improved, the amount of generated wastewater is reduced, the production cost is effectively lowered, and the productivity is greatly improved.

Description

technical field [0001] The invention relates to the field of synthesis of pharmaceutical intermediates, in particular to a production method of N-phenylacetyl-L-glutamine. Background technique [0002] N-phenylacetyl-L-glutamine, molecular weight 264, molecular formula C 13 h 16 N 2 o 4 , the structural formula is . N-phenylacetyl-L-glutamine can be used as a pharmaceutical intermediate and is widely used in the field of pharmaceutical synthesis. The traditional production process of N-phenylacetyl-L-glutamine will generate a large amount of waste water, about 10 kg of waste water will be generated for every 1 kg of product, which greatly increases the pressure of waste water treatment and increases the production cost. Traditional N-phenylacetyl-L-glutamine synthesis steps are long, the yield is low, generally around 60%, the product purity is low, and it is not used in subsequent production. Contents of the invention [0003] The technical problem mainly solved b...

Claims

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Application Information

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IPC IPC(8): C07C237/06C07C231/02
Inventor 刘剑
Owner SUZHOU YUANFANG CHEM