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Preparation method of medical intermediate succinic acid

A technology for succinic acid and intermediates, which is applied in the field of preparation of pharmaceutical intermediates, succinic acid, can solve the problems of low product yield and difficult control conditions, and achieve high product yield, low equipment requirements, and the effect of promoting reaction

Inactive Publication Date: 2019-02-15
嘉兴市秀洲区洪合镇中学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Above-mentioned method condition is more difficult to control, and product yield is lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of pharmaceutical intermediate succinic acid, comprising the following steps:

[0025] (1) Cerium nitrate hexahydrate and copper nitrate are dissolved in particle water to prepare a mixed metal salt solution; wherein, the molar concentrations of each metal ion are respectively: cerium ion 0.55mol / L, copper ion 1.5mol / L;

[0026] (2) Graphene, silane coupling agent and deionized water are mixed, 20min are ultrasonically treated under the power of 500W, and dispersion liquid is obtained; Wherein, the mass ratio of described graphene, silane coupling agent is 1:0.005;

[0027] (3) After mixing and stirring the mixed metal salt solution and dispersion liquid evenly, heat up to 35-45°C, dropwise add sodium hydroxide solution to precipitate while stirring, continue stirring for 1 hour after the dropwise addition, cool to room temperature, filter, filter The final solid was washed with anhydrous ethanol and deionized water in turn, and then directly disper...

Embodiment 2

[0031] A preparation method of pharmaceutical intermediate succinic acid, comprising the following steps:

[0032] (1) Cerium nitrate hexahydrate and copper nitrate are dissolved in particle water to prepare mixed metal salt solution; wherein, the molar concentrations of each metal ion are respectively: cerium ion 1.35mol / L, copper ion 2mol / L;

[0033] (2) Graphene, silane coupling agent and deionized water were mixed, and ultrasonic treatment was performed for 60 min at a power of 1000W to obtain a dispersion; wherein, the mass ratio of graphene and silane coupling agent was 1:0.01;

[0034] (3) After mixing and stirring the mixed metal salt solution and dispersion liquid evenly, heat up to 35-45°C, add dropwise sodium hydroxide solution to precipitate while stirring, continue stirring for 3 hours after the dropwise addition, cool to room temperature, filter, filter The final solid was washed with absolute ethanol and deionized water in turn, and then dispersed directly in cy...

Embodiment 3

[0038] A preparation method of pharmaceutical intermediate succinic acid, comprising the following steps:

[0039] (1) Cerium nitrate hexahydrate and copper nitrate are dissolved in particle water to prepare a mixed metal salt solution; wherein, the molar concentrations of each metal ion are respectively: cerium ion 0.75mol / L, copper ion 1.6mol / L;

[0040] (2) Graphene, silane coupling agent and deionized water were mixed, and ultrasonic treatment was performed for 30min at a power of 600W to obtain a dispersion; wherein, the mass ratio of graphene and silane coupling agent was 1:0.006;

[0041] (3) After mixing and stirring the mixed metal salt solution and dispersion liquid evenly, heat up to 35-45°C, dropwise add sodium hydroxide solution to precipitate while stirring, continue stirring for 1 hour after the dropwise addition, cool to room temperature, filter, filter The final solid was washed with absolute ethanol and deionized water in turn, and then dispersed directly in ...

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PUM

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Abstract

The invention discloses a preparation method of a medical intermediate succinic acid. The preparation method specifically comprises the following steps: first, preparing a compound catalyst accordingto a combination of a coprecipitation method and a sol-gel method, and then preparing a sodium chloride solution, the mass concentration of which is 20-30%; adding acetylpropionic acid and N, N-dimethylformamide into a three-mouth flask with a condensing tube, then adding the sodium chloride solution and a catalyst to be stirred and mixed and slowly heating the mixture to 80-120 DEG C to stir forreaction, and after the reaction, carrying out filtration and collecting a filtrate; adding a hydrochloric acid solution into the filtrate to adjust the pH of the filtrate to 2-3, carrying out filtration, and drying the solid obtained by filtration to prepare succinic acid. The method is simple to operate and high in product yield.

Description

Technical field: [0001] The invention relates to the field of preparation of pharmaceutical intermediates, in particular to a preparation method of the pharmaceutical intermediate succinic acid. Background technique: [0002] Succinic acid, also known as succinic acid, decomposes at 235°C, can be sublimated in vacuum distillation, is soluble in water, slightly soluble in ethanol, ether and acetone. Industrially, succinic acid is often prepared by catalytic reduction of butenedioic acid, and succinic acid can also be prepared by hydrolysis of succinonitrile. In the laboratory, succinic acid can be obtained by reacting two molecules of sodium salt of diethyl malonate with iodine, followed by hydrolytic decarboxylation. Succinic acid has antispasmodic, expectorant and diuretic effects in medicine. Diethyl succinate is an important intermediate in organic synthesis. [0003] Chinese patent (201210339366.2) discloses a method for preparing succinic acid, which uses cellulose-c...

Claims

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Application Information

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IPC IPC(8): C07C51/00C07C55/10B01J23/83
CPCC07C51/00B01J23/002B01J23/83B01J2523/00C07C55/10B01J2523/17B01J2523/3712B01J2523/41B01J2523/47
Inventor 朱胜祥
Owner 嘉兴市秀洲区洪合镇中学