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Preparation method of salazosulfapyridine composition

A technology of sulfasalazine and a compound, which is applied in the field of chemistry to achieve the effect of reducing the tremor phenomenon

Inactive Publication Date: 2020-04-03
SUZHOU HUANGHE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, after long-term use, the elderly over 60 years old with prostate may experience static tremors, and it is necessary to provide a more effective sulfasalazine compound to reduce the tremors of patients

Method used

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preparation example Construction

[0020] The invention provides a preparation method of sulfasalazine compound, comprising the following steps:

[0021] Step 1: adding serine hydrazide hydrochloride and catalyst into an organic solvent, heating and stirring until completely mixed to obtain a mixed solution;

[0022] Step 2: adding trihydroxybenzaldehyde to the mixed solution obtained in step 1, stirring until uniformly mixed, as a precursor solution;

[0023] Step 3: Adding thick sulfasalazine to the precursor solution for hydrogenation, after the hydrogenation is completed, the organic solvent is evaporated at low temperature and an extractant is added to extract the crystal;

[0024] Step 4: washing the crystals with ethanol to obtain a sulfasalazine compound.

[0025] Specifically, in the first step, the mass ratio of serine hydrazide hydrochloride to the catalyst is 1:0.3-0.6, and the organic solvent is an alcoholic organic solvent. Preferably, the catalyst is a metal catalyst. Further, in step 1, the h...

Embodiment 1

[0031] Add 10g of serine hydrazide hydrochloride and 5g of the metal catalyst into the glycerol solution, heat to 60°C and stir for 3 hours until completely mixed to obtain a mixed solution; add trihydroxybenzaldehyde to the mixed solution obtained in step 1, and mix The mass ratio of the solution to trihydroxybenzaldehyde is 1:1. Further, the reaction pressure is controlled to 0.75mpa, the temperature is 10±5°C, stirred until the mixture is even, and used as a precursor solution; The precursor solution is heated to 25±2°C, and the organic solvent is evaporated at low temperature. After the reaction pressure is constant, ethanol is added to the reaction solution to extract the crystal; the extracted crystal is washed with ethanol for 6 times, and the washed crystal is dried. Dry and crush to obtain the sulfasalazine compound.

Embodiment 2

[0033] Add 15g of serine hydrazide hydrochloride and 4.5g of metal catalyst into the ethanol solution, heat to 60°C and stir for 2.5h until completely mixed to obtain a mixed solution; add trihydroxybenzaldehyde to the mixed solution obtained in step 1, and mix The mass ratio of the solution to trihydroxybenzaldehyde is 1:1.2. Further, the reaction pressure is controlled to 0.8mpa, the temperature is 10±5°C, and it is stirred until it is evenly mixed as a precursor solution; The temperature of the precursor solution was raised to 24±1°C, and the precursor solution was added to the crude sulfasalazine to mix according to the mass ratio of 1:45; the organic solvent was evaporated at low temperature, and after the reaction pressure was constant, acrylic acid was added to the reaction solution. Alcohol extraction of the crystals; washing the extracted crystals with ethanol for 5 times, drying and crushing the washed crystals to obtain the sulfasalazine compound.

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Abstract

The invention provides a preparation method of a salazosulfapyridine composition. The preparation method of the salazosulfapyridine composition comprises the following steps: step 1, adding serine hydrazide hydrochloride and a catalyst into an organic solvent, and heating and stirring until the serine hydrazide hydrochloride and the catalyst are completely mixed to obtain a mixed solution; step 2,adding trihydroxybenzaldehyde into the mixed solution obtained in the step 1, and stirring until the trihydroxybenzaldehyde and the mixed solution are uniformly mixed to obtain a precursor solution;step 3, hydrogenating the precursor solution, adding a salazosulfapyridine crude body, mixing, evaporating to remove the organic solvent at a low temperature after hydrogenation is finished, and adding an extracting agent to extract crystals; and step 4, washing the crystal with ethanol or acetone to obtain the salazosulfapyridine composition. The preparation method of the salazosulfapyridine composition is simple in preparation process and suitable for popularization and application.

Description

technical field [0001] The invention provides a preparation method of a sulfasalazine compound, which belongs to the technical field of chemistry. Background technique [0002] Sulfasalazine is a sulfonamide antibacterial drug. It is a sulfa drug that is not easy to absorb when taken orally. The absorbed part is decomposed into 5-aminosalicylic acid and sulfapyridine under the action of intestinal microorganisms. 5-aminosalicylic acid complexes with the connective tissue of the intestinal wall and stays in the intestinal wall tissue for a long time to play an antibacterial, anti-inflammatory and immunosuppressive role, such as reducing Escherichia coli and Clostridium and inhibiting the synthesis of prostaglandins and the synthesis of other inflammatory mediators leukotrienes. Therefore, it is currently believed that the main component of this product to produce curative effect on inflammatory bowel disease is 5-aminosalicylic acid. [0003] However, after long-term use, ...

Claims

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Application Information

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IPC IPC(8): C07D213/76
CPCC07B2200/13C07D213/76
Inventor 肖祖华江尔胜
Owner SUZHOU HUANGHE PHARMA CO LTD
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