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A novel ubenimex recrystallization method

A technology for ubimethoxine and ubimethoxine hydrochloride, which is applied in the field of medicine, can solve the problems that the overall yield does not meet the production requirements, the agitator motor is easily damaged, and the agitator cannot operate, and the production process is easy to control and increase. Yield, the effect of avoiding agglomeration

Active Publication Date: 2020-06-12
SHANGHAI SINE WANXIANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses the crystallization method of one-way dropwise addition. When the pH of the system is 2 to 4, intermolecular polymers will be formed, which will cause instant agglomeration. It cannot continue, and it is easy to damage the agitator motor. At this time, it is necessary to add a large amount of purified water to dissolve the agglomerates before continuing production, which will reduce the yield.
[0004] At the same time, Chinese patent CN103360277A also discloses a method for recrystallization of ubenimex, which is to drop ubenimex hydrochloride solution and alkali solution into the recrystallization container at the same time, and control the dropping rate to keep the pH value of the system at 3-6, and then crystallized and filtered to obtain the refined product of ubenimex. Although the purity of ubenimex has been improved to a certain extent by this method, there is still the problem of partial agglomeration, which affects the production process, and its The overall yield did not meet the production requirements and needs further in-depth research

Method used

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  • A novel ubenimex recrystallization method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Add 1000ml of sodium dihydrogen phosphate / disodium hydrogen phosphate buffer solution with a pH value of 7 into a three-necked flask, add 350 g of Ubenimex crude product, stir, heat to a temperature of 60°C, and dropwise add 102 ml of 18.5% hydrochloric acid solution , the crude product was completely dissolved and filtered to obtain Ubenimex hydrochloric acid solution;

[0030] (2) Get another three-necked flask and add 2000ml of purified water, control the temperature of the system in an ice-water bath below 4°C, add dropwise ubenimex hydrochloric acid solution and 5% ammonia water at the same time, control the dropping speed of the two solutions, and make the pH of the reaction system value was kept at 5-7, the dropwise addition of the ubenimex hydrochloric acid solution was completed, the amount of ammonia water was added dropwise to 74ml, stirred and crystallized for 15h, filtered to obtain a filter cake;

[0031] (3) Filter cake The filtered filter cake was wa...

Embodiment 2

[0033] (1) Add 1000ml of sodium dihydrogen phosphate / disodium hydrogen phosphate buffer solution with a pH value of 7 into a three-neck flask, add 350 g of Ubenimex crude product, and add 1.7 g of sodium chloride solid, stir, and heat to a temperature of 60°C , 96ml of 18.5% hydrochloric acid solution was added dropwise, the crude product was completely dissolved, filtered to obtain ubenimex hydrochloric acid solution;

[0034] (2) Get another three-necked flask and add 2000ml of purified water, control the temperature of the system in an ice-water bath below 4°C, add dropwise ubenimex hydrochloric acid solution and 5% ammonia water at the same time, control the dropping speed of the two solutions, and make the pH of the reaction system value was kept at 5-7, the dropwise addition of the ubenimex hydrochloric acid solution was completed, the amount of ammonia water added was 77ml, stirred and crystallized for 15 hours, filtered to obtain a filter cake;

[0035] (3) Filter cake...

Embodiment 3

[0037] (1) Add 1000ml of sodium dihydrogen phosphate / disodium hydrogen phosphate buffer solution with a pH value of 7 into a three-necked flask, add 350g of Ubenimex crude product, and add 3.5g of sucrose, stir, heat to a temperature of 60°C, add dropwise 80ml of 18.5% hydrochloric acid solution, the crude product was completely dissolved, filtered to obtain ubenimex hydrochloric acid solution;

[0038] (2) Get another three-necked flask and add 2000ml of purified water, control the temperature of the system in an ice-water bath below 4°C, add dropwise ubenimex hydrochloric acid solution and 5% ammonia water at the same time, control the dropping speed of the two solutions, and make the pH of the reaction system value was kept at 5-7, the dropwise addition of the ubenimex hydrochloric acid solution was completed, the amount of ammonia water was added dropwise to 61ml, stirred and crystallized for 15h, filtered to obtain a filter cake;

[0039] (3) Filter cake The filtered filt...

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Abstract

The invention discloses a novel ubenimex recrystallization method. According to the method, PH is controlled in a manner of bidirectionally, simultaneously and dropwise adding an ubenimex acid solution and an alkali solution, and a PH buffer solution is used as a dispersion system, so that PH control is more accurate, the problem that agglomerates are easy to produce in the prior art is solved, the production process is easy to control, the quality is stable, the yield is also increased, the usage quantity of an ammonia solution and the usage quantity of hydrochloric acid are reduced, the cost is reduced, besides, the generation of three wastes is also reduced, the total yield is increased, and besides, the novel ubenimex recrystallization method is environmentally-friendly.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a novel recrystallization method 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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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C237/20
CPCC07C231/24C07C237/20
Inventor 朱婷媛顾煜刘瀛
Owner SHANGHAI SINE WANXIANG PHARMA
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