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Preparation method of hydrocortisone sodium succinate

A technology of hydrocortisone sodium succinate and hydrocortisone, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry, steroids, etc., and can solve the problems of high impurity content in products, difficult processing, and complicated processing operations and other issues, to achieve the effect of good product quality, low impact on the environment and human body, and high product purity

Inactive Publication Date: 2019-07-05
ZHENGZHOU MINGZE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The impurity content of the prepared product is high, and the post-processing is difficult and the processing operation is complicated

Method used

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Examples

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preparation example Construction

[0026] In one embodiment of the invention, the invention provides a kind of preparation method of hydrocortisone sodium succinate, the method comprises the following steps:

[0027] (1) Take succinic anhydride and hydrocortisone as raw materials, dissolve them in a solvent, and react for 4-8 hours at 45-60°C in the presence of a catalyst to obtain a reaction solution

[0028] In this step, the solvent is tetrahydrofuran and / or N,N-dimethylformamide; the mass volume ratio of the succinic anhydride to the solvent is 1 g: (1.0-10.0) ml; typical but non-limiting mass volume The ratio is 1g: 1.0ml, 1g: 2.0ml, 1g: 3.0ml, 1g: 4.0ml, 1g: 5.0ml, 1g: 6.0ml, 1g: 7.0ml, 1g: 8.0ml, 1g: 9.0ml, 1g: 10.0 ml.

[0029] In this step, the molar ratio of hydrocortisone to succinic anhydride is 1:1.5-2.5, and the typical but non-limiting molar ratios are 1:1.5, 1:2.0, 1:2.5;

[0030] In this step, the mass ratio of the succinic anhydride to the catalyst is 1:0.001 to 0.1; typical but non-limiting...

Embodiment 1

[0043] (1) Add 45g succinic anhydride, 250ml N,N-dimethylformamide (DMF) and 250ml tetrahydrofuran (THF) mixed solvent, 110g hydrocortisone, 10g 4-dimethylamino Pyridine (DMAP), heated to 45°C in a water bath, magnetically stirred until the solution was clear, and stirred for 4 hours at 45°C to complete the reaction to obtain a reaction solution;

[0044] (2) Add 250ml of acetone to the reaction solution obtained in step (1) (acetone makes the precipitated product not agglomerate. Because the polarity of acetone is between DMF / THF and water, it can level the polarity of the reaction solution and the polarity of water , so that the product is better separated out, avoiding agglomeration and product state) stirring evenly to obtain the mixed solution, cooling the temperature of the mixed solution to below 10°C, and then adding 35 times the weight of succinic anhydride in the mixed solution in the mixed solution Purified water (the temperature of purified water is 0-5°C), crystal...

Embodiment 2

[0047] (1) Add 60g of succinic anhydride, 300ml of N,N-dimethylformamide (DMF) and 300ml of tetrahydrofuran (THF) mixed solvent, 110g of hydrocortisone, 10g of 4-dimethylamino Pyridine (DMAP), heated to 45°C in a water bath, magnetically stirred until the solution was clear, and stirred for 4 hours at 45°C to complete the reaction to obtain a reaction solution;

[0048] (2) Add 300ml of acetone to the reaction solution obtained in step (1) and stir evenly to obtain a mixed solution, cool the temperature of the mixed solution to below 10°C, and then add 35% succinic anhydride with a weight equivalent to the weight of succinic anhydride in step (1) to the mixed solution. times of purified water (the temperature of purified water is 0-5°C), crystallize at 0-5°C for 2 hours under stirring conditions, filter, and dry the obtained crystals at 60°C to constant weight to obtain hydrocortisone amber Acid monoester; After testing, the obtained hydrocortisone succinate monoester fine pro...

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Abstract

The invention discloses a preparation method of hydrocortisone sodium succinate. The method comprises the steps of preparing hydrocortisone succinic acid monoester by using succinic anhydride and hydrocortisone as raw materials; and performing a reaction by using the hydrocortisone succinic acid monoester as a raw material at a low temperature, and after the reaction is completed, performing treatment on the reaction liquid by adopting acetone with a temperature of about -20 DEG C to obtain the hydrocortisone sodium succinate. The process conditions adopted in the method provided by the invention are as follows: the sodium salt is generated at the low temperature, then the reaction liquid is added into a large amount of acetone, filtering is performed, the filter cake is washed by using the acetone and water, and finally vacuum drying is performed to remove the acetone; the process of high-temperature steaming is avoided, so that the product is stable, and has a high yield and a good state; the purity can reach 97% or more during reaction, and after purification, the product is in full compliance with the Chinese Pharmacopoeia standard; and the acetone can be recycled, so that theproduction costs are saved; therefore, the solution is suitable for industrial production, and the product quality is good.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of hydrocortisone sodium succinate. Background technique [0002] Hydrocortisone sodium succinate is used to rescue critically ill patients, such as toxic infection, anaphylactic shock, severe adrenal cortex hypofunction, connective tissue disease, severe bronchial asthma and other allergic diseases, and can be used to prevent and treat transplantation An adrenal corticosteroid drug for acute rejection. During the use of this drug, it will not bring side effects such as facial flushing, excitement, irritability, and increased heart rate caused by traditional hydrocortisone alcohol-based preparations to patients, and hydrocortisone sodium succinate is a water-soluble instant preparation. Fast absorption, rapid action, very suitable for clinical application. Therefore, the market application of hydrocortisone sodium succinate is very wi...

Claims

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Application Information

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IPC IPC(8): C07J5/00C07C51/43C07C55/10
CPCC07C51/43C07J5/0053C07C55/10
Inventor 徐元程苗苗徐贡杰
Owner ZHENGZHOU MINGZE MEDICAL TECH
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