Method for recovering bezafibrate from bezafibrate synthesis waste liquid

A technology of bezafibrate and waste liquid is applied in the field of drug synthesis, which can solve the problems of stickiness and blackening, increase production cost, difficulty in recycling and the like, and achieve the effects of high purity of crude product and simple and easy operation method.

Inactive Publication Date: 2018-04-10
JIANGSU HEALTH VOCATIONAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic waste liquid also contains a relatively high content of bezafibrate, but because the waste liquid contains a lot of condensation reaction side reaction impurities, it is sticky and black, and it is very difficult to recycle, so it can only be thrown away as waste liquid, increasing cost of production
[0003] After searching, there is no prior art that discloses a practical method for recovering the remaining bezafibrate from waste liquid

Method used

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  • Method for recovering bezafibrate from bezafibrate synthesis waste liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Take 100mL of synthetic waste liquid, add 1L of water to dissolve and dilute, and pass CO into it at a rate of 200mL / min 2 After 30 minutes, add 15 mL of chitosan solution with a mass concentration of 1%, flocculate at room temperature for 30 minutes, and suction filter; then add 22 g of chitosan / attapulgite complex to the obtained filtrate, stir at room temperature for 15 minutes, and let stand for 30 minutes , after suction filtration, the filtrate was acidified with 15% hydrochloric acid to pH=3.5, stirred at room temperature for 1 h until the precipitation was complete, filtered, and the filter cake was dried to obtain 25 g of crude bezafibrate.

[0024] The preparation method of the 1% chitosan solution is as follows: 1 g of chitosan is dissolved in 100 mL of 1% acetic acid aqueous solution with a mass fraction.

[0025] The chitosan / attapulgite composite was prepared by the following method: 1 g of chitosan was dissolved in 100 mL of 1% acetic acid aqueous solutio...

Embodiment 2

[0027] Take 500mL of synthetic waste liquid, add 2.5L of water to dissolve and dilute, and pass CO into it at a rate of 200mL / min 2 After 20 minutes to pH 5, add 60 mL of chitosan solution with a mass concentration of 1%, suction filter after flocculation at room temperature for 20 minutes; After filtration, the filtrate was acidified with 15% hydrochloric acid to pH = 3, stirred at room temperature for 1 h until the precipitation was complete, filtered, and the filter cake was dried to obtain 102 g of crude bezafibrate.

[0028] The preparation method of the 1% chitosan solution is as follows: 1 g of chitosan is dissolved in 100 mL of 1% acetic acid aqueous solution with a mass fraction.

[0029] The chitosan / attapulgite composite was prepared by the following method: 1 g of chitosan was dissolved in 100 mL of 1% acetic acid aqueous solution to obtain a chitosan sol, 6 g of attapulgite was added to the sol and stirred continuously at room temperature for 48 h After standing ...

Embodiment 3

[0031] Take 1L of synthetic waste liquid, add 15L of water to dissolve and dilute, and pass CO into it at a rate of 200mL / min 2 To pH 6, after 40 minutes, add 160 mL of chitosan solution with a mass concentration of 1%, suction filter after 30 minutes of flocculation at room temperature; After suction filtration, the filtrate was acidified with 15% hydrochloric acid to pH=4, stirred at room temperature for 1 h until the precipitation was complete, filtered, and the filter cake was dried to obtain 225 g of crude bezafibrate.

[0032] The preparation method of the 1% chitosan solution is as follows: 1 g of chitosan is dissolved in 100 mL of 1% acetic acid aqueous solution with a mass fraction.

[0033] The chitosan / attapulgite composite was prepared by the following method: 1 g of chitosan was dissolved in 100 mL of 1% acetic acid aqueous solution to obtain a chitosan sol, 6 g of attapulgite was added to the sol and stirred continuously at room temperature for 48 h After standi...

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Abstract

The invention discloses a method for recovering bezafibrate from bezafibrate synthetic waste liquid, wherein the synthetic waste liquid refers to N-p-hydroxyphenethyl-4-chlorobenzamide, acetone and chloroform in alkaline The mother liquor after condensation and precipitation of crude bezafibrate under conditions, and the remaining acetone in the mother liquor has been recovered, including dilution with water, flocculation adsorption and acidification crystallization; wherein, flocculation adsorption is carried out under weakly acidic conditions, flocculation adsorption material At least chitosan is included; preferably, chitosan/attapulgite complex is also included. In short, the method provided by the present invention not only uses a low-cost green material for separation, but also has a simple and easy operation method, which is suitable for large-scale industrial production, and is a green and low-cost method, which can effectively remove bezabe The high-purity crude bezafibrate is recovered from the specially synthesized waste liquid, thereby reducing the production cost.

Description

technical field [0001] The invention belongs to the field of drug synthesis and relates to the recycling of synthetic waste liquid, in particular to a method for recovering bezafibrate from bezafibrate synthetic waste liquid. Background technique [0002] Bezafibrate is a fibrate blood lipid regulating drug widely used clinically. At present, the synthesis of bezafibrate bulk drug mainly uses tyramine as raw material, obtains N-p-hydroxyphenethyl-4-chlorobenzamide through acylation, and then reacts with chloroform and acetone under alkaline conditions (usually with NaOH) The next condensation, and finally derived from crystallization. The mother liquor after crystallization recovers the remaining acetone and treats it as synthetic waste liquid. The synthetic waste liquid also contains a relatively high content of bezafibrate, but because the waste liquid contains a lot of condensation reaction side reaction impurities, it is sticky and black, and it is very difficult to re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/73C07C231/24C07C231/12
CPCC07C231/24C07C231/12C07C233/73
Inventor 吴洁鲍真真王素珍
Owner JIANGSU HEALTH VOCATIONAL COLLEGE
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