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Method for recrystallizing ubenimex

A technology of ubenimex and ubenimex hydrochloride, which is applied in the field of medicine and can solve problems such as production failure, agitator failure, and yield reduction

Inactive Publication Date: 2013-10-23
SHANGHAI SINE WANXIANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, when the pH of the system is around 2.5, the material will instantly agglomerate, and the agglomeration will cause the agitator to fail to operate, so that the production cannot continue, and it is also easy to damage the agitator motor. At this time, a large amount of purified water needs to be added. Agglomerates must be redissolved to continue production, which reduces yield

Method used

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  • Method for recrystallizing ubenimex
  • Method for recrystallizing ubenimex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 1000ml of purified water into the three-necked flask, start stirring, add 350g of crude ubenimex, heat to 60±2°C, add hydrochloric acid (18.5%) dropwise until the crude product dissolves, filter to obtain ubenimex hydrochloric acid solution.

[0012] Take another three-neck flask and add 2000ml of purified water, start stirring, control the temperature of the system at about 0°C in an ice-water bath, and add ubenimex hydrochloric acid solution and ammonia water (4%) dropwise at the same time, control the dropping speed of the two solutions, and make the reaction system The pH is maintained around 3-4. After the acid solution is added dropwise, use ammonia water (1%) to fine-tune the pH=5-6, and filter after 24 hours of crystallization.

[0013] The filter cake was washed with a small amount of purified water, filtered with suction until there was no water drop, and dried under reduced pressure at 40°C to constant weight. The purity of the product was tested to be 99...

Embodiment 2

[0015] Add 1000ml of purified water into a three-neck flask, start stirring, add 350g of crude ubenimex, heat to 60±2°C, add hydrochloric acid (18.5%) dropwise until the crude product dissolves, filter to obtain ubenimex hydrochloric acid solution.

[0016] Take another three-neck flask and add 2000ml of purified water, start stirring, and control the temperature of the system at about 2°C in an ice-water bath. The pH is maintained around 4-5. After the acid solution is added dropwise, use ammonia water (1%) to fine-tune the pH=5-6, and filter after 24 hours of crystallization.

[0017] The filter cake was washed with a small amount of purified water, filtered with suction until there was no water drop, and dried under reduced pressure at 40°C to constant weight. The purity of the product was tested to be 100.2%, and the total yield was 90.3%.

Embodiment 3

[0019] Add 1000ml of purified water into the three-necked flask, start stirring, add 350g of crude ubenimex, heat to 60±2°C, add hydrochloric acid (18.5%) dropwise until the crude product dissolves, filter to obtain ubenimex hydrochloric acid solution.

[0020] Take another three-neck flask and add 2000ml of purified water, start stirring, and control the temperature of the system at about 3°C ​​in an ice-water bath. The pH is maintained around 3-4. After the acid solution is added dropwise, use ammonia water (1%) to fine-tune the pH=5-6, and filter after 24 hours of crystallization.

[0021] The filter cake was washed with a small amount of purified water, filtered with suction until there was no water drop, and dried under reduced pressure at 40°C to constant weight. The purity of the product was tested to be 99.6%, and the total yield was 91.1%.

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Abstract

The invention belongs to the technical field of medicines and in particular relates to a method for recrystallizing ubenimex. By adopting the method for recrystallizing ubenimex, the phenomenon that materials can be instantly caked in the existing ubenimex crude product recrystallization process is avoided, hydraulic acid and ammonia water are greatly saved, and the total yield is increased by about 7-8 percent points.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for recrystallization of ubenimex. Background technique [0002] Ubenimex is a compound isolated from the culture fluid of Streptomycesoforecticuli, which can competitively inhibit aminopeptidase B (aminopeptidaseN / CD13) and leucineamino-peptidase (Leucineamino-Peptidase). Ubenimex can enhance the function of T cells, enhance the killing activity of NK cells, and increase the synthesis of colony-stimulating factor to stimulate the regeneration and differentiation of bone marrow cells. This product can interfere with the metabolism of tumor cells, inhibit tumor cell proliferation, cause tumor cell apoptosis, activate human cellular immune function, stimulate the production and secretion of cytokines, promote the production and proliferation of anti-tumor effector cells, and be used for anti-cancer chemotherapy , Adjuvant therapy of radiotherapy, senile immunodeficiency,...

Claims

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Application Information

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IPC IPC(8): C07C237/20C07C231/24
Inventor 刘瀛顾煜
Owner SHANGHAI SINE WANXIANG PHARMA
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