Process for removing pidotimod condensation impurities

A technology of pidotimod and impurities, applied in the preparation method of peptides, organic chemistry, peptides, etc., can solve the problems of no removal, no removal process, and inability to guarantee product quality, so as to shorten cycle time and ensure quality Effect

Active Publication Date: 2018-05-08
BEIJING JINCHENG TAIER PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Patent CN102952172A and patent CN102167727A also use DCC as condensing agent, but they also do not involve the method of removing DCU dissolved in the mother liquor, so the quality of the product cannot be guaranteed
[0006] In summary, the existing process of producing pidotimod using DCC as a condensing agent is the process with the best yield and quality, and is also the most environmentally f

Method used

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  • Process for removing pidotimod condensation impurities

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Weigh 100g of dichloromethane and pump it into a 200mL reaction flask, stir, add 17g of L-thiazolidine-4-carboxylic acid ethyl ester hydrochloride, add 20g of purified water, start to add 4.0g of sodium carbonate solid, react for 30 minutes, static Set aside for 30 minutes, separate layers, temporarily store the dichloromethane layer; stir, add 11.3g L-pyroglutamic acid, add 15g DCC dropwise, take 4 hours, dropwise addition is complete, keep warm for 10 hours, keep warm, start to filter DCU , suction filtered until there is basically no filtrate, then rinse twice with 20g*2 dichloromethane, add the above dichloromethane solution into a 500mL reaction flask, add 40g of purified water, start to add 28g of sodium hydroxide aqueous solution dropwise, drop Completed, heat-insulated and stirred for 3 hours, left to stand for 30 minutes, separated into layers, the upper aqueous layer was a yellow liquid, liquid-separated, and the aqueous phase was retained to obtain an aqueous ...

Embodiment 2

[0036] Weigh 100g of dichloromethane and pump it into a 200mL reaction flask, stir, add 17g of L-thiazolidine-4-carboxylic acid ethyl ester hydrochloride, add 20g of purified water, start to add 4.0g of sodium carbonate solid, react for 30 minutes, static Set aside for 30 minutes, separate layers, temporarily store the dichloromethane layer; stir, add 11.3g L-pyroglutamic acid, add 15g DCC dropwise, take 4 hours, dropwise addition is complete, keep warm for 10 hours, keep warm, start to filter DCU , suction filtered until there is basically no filtrate, then rinse twice with 20g*2 dichloromethane, add the above dichloromethane solution into a 500mL reaction flask, add 40g of purified water, start to add 28g of sodium hydroxide aqueous solution dropwise, drop Completed, heat-insulated and stirred for 3 hours, left to stand for 30 minutes, separated into layers, the upper aqueous layer was a yellow liquid, liquid-separated, and the aqueous phase was retained to obtain an aqueous ...

Embodiment 3

[0039] Weigh 100g of dichloromethane and pump it into a 200mL reaction flask, stir, add 17g of L-thiazolidine-4-carboxylic acid ethyl ester hydrochloride, add 20g of purified water, start to add 4.0g of sodium carbonate solid, react for 30 minutes, static Set aside for 30 minutes, separate layers, temporarily store the dichloromethane layer; stir, add 11.3g L-pyroglutamic acid, add 15g DCC dropwise, take 4 hours, dropwise addition is complete, keep warm for 10 hours, keep warm, start to filter DCU , suction filtered until there is basically no filtrate, then rinse twice with 20g*2 dichloromethane, add the above dichloromethane solution into a 500mL reaction flask, add 40g of purified water, start to add 28g of sodium hydroxide aqueous solution dropwise, drop Completed, heat-insulated and stirred for 3 hours, left to stand for 30 minutes, separated into layers, the upper aqueous layer was a yellow liquid, liquid-separated, and the aqueous phase was retained to obtain an aqueous ...

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Abstract

The invention relates to pidotimod, in particular to a process for removing pidotimod condensation impurities. The process for removing the pidotimod condensation impurities includes the step of preparing dichloromethane mother liquor containing dicyclohexylurea in a process for preparing pidotimod. According to the process for preparing pidotimod, dicyclohexyl carbodiimide serves as a condensingagent, the dichloromethane mother liquor containing dicyclohexylurea is subjected to hydrolysis and skimming, a water phase is obtained, the water phase is treated through a macroporous resin filler column, salification is achieved after the water phase is treated, and pidotimod is obtained after refining is carried out. The dichloromethane mother liquor containing dicyclohexylurea is subjected tohydrolysis and skimming, the water phase is obtained, the water phase is treated through the macroporous resin filler column, and the impurities, namely dicyclohexylurea, in pidotimod products are completely removed. The defect that the impurities, namely dicyclohexylurea cannot be completely removed through an existing process is overcome, and the method which is simple, effective, safe, environmentally friendly and suitable for industralization is found.

Description

technical field [0001] The invention relates to pidotimod, in particular to a process for removing condensed impurities of pidotimod. Background technique [0002] Pidotimod was developed by an Italian company and obtained a clinical immune booster in 1992, which can promote both non-specific and specific immune responses. Pidotimod can strengthen the phagocytic activity of macrophages and neutrophils, improve their chemotaxis; activate natural killer cells, promote the proliferation of lymphocytes caused by mitogens, and make helper T cells (CD4+) with low immune function Ratio to suppressor T cells (CD8+) increases and returns to normal; promotes cellular immune response by stimulating interleukin-a and r-interferon. In fact, pidotimod has no direct antibacterial and antiviral activity, but it exerts significant antibacterial and antiviral effects by promoting the immune function of the body. Clinically, it is mainly used for recurrent respiratory tract infection and uri...

Claims

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Application Information

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IPC IPC(8): C07K5/078C07K1/12C07K1/02
CPCC07K5/06139
Inventor 张彤孙滨许蕾周海洋马庆双王晓光
Owner BEIJING JINCHENG TAIER PHARMA CO LTD
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