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Synthesis method of phthaloyl alanyl glutamine

A technology of phthaloyl alanyl glutamine and a process method, applied in the direction of peptides and the like, can solve the problems of complex process, high cost, and high three wastes, and achieve controllable stability, reduction of recovery cost, and cost reduction. Effect

Inactive Publication Date: 2017-07-14
JIANGSU CHENGXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the synthesis process of phthalylalanyl glutamine is complicated, the cost is high, and the three wastes are high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A synthetic process for phthalylalanyl glutamine, comprising the steps of:

[0039] A. Synthesis of Intermediate I

[0040] 1) Add toluene, phthalic anhydride and L-alanine into the reaction kettle and stir well. Wherein the feeding amount of toluene is 200-300g / L, the feeding amount of phthalic anhydride is 140-150g / L, and the feeding amount of L-alanine is 80-90g / L;

[0041] 2) Heat up to 100-130°C to reflux and divide water, and keep warm for about 2-6 hours;

[0042] 3) Cool down to 70-90°C, add toluene 100-200g / L, cool down to 0-30°C, stir and crystallize for 5-15h;

[0043] 4) After the crystallization is completed, discharge and centrifuge, reduce pressure at 50-80°C, vacuum degree ≤ -0.09MPa, and dry for 6-8 hours to obtain Intermediate I;

[0044] B. Synthesis of Intermediate 2

[0045] 1) Add the intermediate 1 prepared in the above steps to the reaction kettle, and stir the thionyl chloride evenly; the feeding amount of the intermediate 1 is 180-250g / L, a...

Embodiment 2

[0058] Embodiment 2: intermediate I synthesis

[0059] 1. Add 110g of toluene, 71g of phthalic anhydride and 40g of L-alanine into a 500mL three-neck flask equipped with a cooling reflux water separation device, stir evenly, raise the temperature to 105-110°C to reflux water separation, and keep warm for about 3 Hour;

[0060] 2. Cool down to 70-75°C, add 50g of toluene, continue to cool down to 0-5°C, stir and crystallize for 5h;

[0061] 3. After the crystallization is completed, filter and dry the wet product at 50-55°C under reduced pressure (vacuum degree ≤ -0.09MPa) for 6-8 hours to obtain intermediate I95g, yield: 96.9%.

Embodiment 3

[0062] Embodiment 3: intermediate I synthesis

[0063] 1. Add 120g of toluene, 73g of phthalic anhydride and 41g of L-alanine into a 500mL three-necked flask equipped with a cooling reflux water separation device, stir evenly, raise the temperature to 110-115°C to reflux water separation, and keep warm for about 4 Hour;

[0064] 2. Cool down to 70-75°C, add 60g of toluene, continue to cool down to 10-15°C, stir and crystallize for 8h;

[0065] 3. After the crystallization is completed, filter and depressurize the wet product at 60-65°C, vacuum degree ≤ -0.09MPa, and dry for 6-8 hours to obtain intermediate I98g, yield: 97.2%.

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PUM

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Abstract

The invention provides a synthesis method of phthaloyl alanyl glutamine. According to the synthesis method, methylbenzene, phthalic anhydride, and L-alanine are taken as starting materials, and synthesis of an intermediate I, an intermediate II, a phthaloyl alanyl glutamine crude product, and phthaloyl alanyl glutamine are realized. The synthesis method is low in production cost, mild in reaction conditions, and simple in operation, and is controllable; using of a large amount of toxic reagents is avoided; the synthesis method is safe, and is friendly to the environment; and product quality is stable.

Description

technical field [0001] The invention relates to a process for synthesizing phthalylalanyl glutamine, which belongs to the technical field of medicine and its intermediates. Background technique [0002] Phthalylalanylglutamine is an important intermediate of alanylglutamine. Alanylglutamine is mainly used in parenteral and enteral nutritional supplements for surgical trauma. It is widely used in the treatment and rapid recovery of trauma, major surgery, large area burns, chemical poison injuries, and radiation injuries. It plays an important role in the treatment and recovery of patients with large area sudden trauma, malignant tumor, chemical poison injury, radiation injury and pest injury. The synthesis process of phthalylalanyl glutamine has influenced the industry and application of alanyl glutamine. In the prior art, the process for synthesizing phthalylalanyl glutamine is complex, high in cost and high in three wastes. Contents of the invention [0003] Purpose of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/062C07K1/02
Inventor 吴锋祝俊刘家生华俊国王峰峰邢飞许昇何宝亮
Owner JIANGSU CHENGXIN PHARMA
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