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A method of preparing medicinal magnesium acetate tetrahydrate

A magnesium acetate, medicinal technology, applied in the direction of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve problems such as inability to use and products that do not meet the quality standard requirements, and achieve cost saving and convenient storage , The effect of short process flow

Inactive Publication Date: 2017-02-08
HUAREN PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention provides a method for preparing medicinal magnesium acetate tetrahydrate, which solves the problem in the prior art that the product obtained by the preparation method of magnesium acetate tetrahydrate does not meet the requirements of quality standards and cannot be used

Method used

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  • A method of preparing medicinal magnesium acetate tetrahydrate

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Effect test

Embodiment 1

[0028] In the reaction flask, add glacial acetic acid 216.2g (2.1 molar equivalent), water 800mL, start mechanical stirring, add magnesium hydroxide 100g (1 molar equivalent), then, heat to 75°C for 1 hour, and cool the reaction solution to room temperature; Adjust the pH value of the solution to 7.70 with magnesium hydroxide, filter, and adjust the pH of the filtrate to 5.22 with glacial acetic acid; the solution is concentrated under reduced pressure, and the density of the concentrated solution is detected. When the density reaches 1.283, the concentration is stopped, and the concentrated solution is stirred at room temperature Crystallization; after about 6 hours of crystallization, filter, and wash the filter cake with 100 mL of absolute ethanol; finally, place it in a blast drying oven at 50°C for 3 hours to obtain the finished product.

Embodiment 2

[0030] In the reaction flask, add glacial acetic acid 216.2g (2.1 molar equivalent), water 800mL, start mechanical stirring, add magnesium hydroxide 100g (1 molar equivalent), then heat to 80°C for 0.5h, and cool the reaction solution to 35°C Below; use magnesium hydroxide to adjust the pH value of the solution to 8.31, filter, and use glacial acetic acid to adjust the pH of the filtrate to 5.21; this solution is concentrated under reduced pressure, and the density of the concentrated solution is detected. When the density reaches 1.284, stop concentrating and leave the concentrated solution at room temperature Stir and crystallize at low temperature; after 5 hours of crystallization, filter, and wash the filter cake with 100 mL of absolute ethanol; finally, place it in a blast drying oven at 50°C for 4 hours to obtain the finished product.

Embodiment 3

[0032] In the reaction flask, add glacial acetic acid 216.2g (2.1 molar equivalent), water 800mL, start mechanical stirring, add magnesium hydroxide 100g (1 molar equivalent), then heat to 78°C, react for 1.5h, and cool the reaction liquid to 25 ℃; use magnesium hydroxide to adjust the pH value of the solution to 9.0, filter, and use glacial acetic acid to adjust the pH value of the filtrate to 5.22; this solution is concentrated under reduced pressure, and the temperature during the reduced pressure concentration is 80°C, and the density of the concentrated solution is detected. When the concentration reaches 1.281, the concentration is stopped, and the concentrated solution is stirred and crystallized at room temperature; after 7 hours of crystallization, filter, and the filter cake is washed with 100 mL of absolute ethanol; finally, it is placed in a blast drying oven at 55°C for 2 hours to obtain the finished product .

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Abstract

A method of preparing medicinal magnesium acetate tetrahydrate is disclosed and belongs to the technical field of chemical bulk drug synthesis. The method includes steps of 1) weighing analytically pure magnesium hydroxide and analytically pure glacial acetic acid, adding water, heating to 75-80 DEG C, and cooling to 35 DEG C or below after the reaction is finished, 2) adjusting the pH value to 7.7-9.0 by adopting the magnesium hydroxide, filtering, and adjusting the pH value of the filtrate to 4.8-5.7 by adopting the glacial acetic acid to obtain a solution, 3) performing vacuum concentration until the density of the concentrate is 1.250-1.310, and crystallizing under stirring, 4) filtering and washing and 5) performing air blast drying to obtain a finished product. Through strictly controlling the pH value of the reaction solution, the pH value of the filtrate and the density before crystallization, the prepared magnesium acetate tetrahydrate reaches magnesium acetate tetrahydrate quality standards in the European Pharmacopoeia, and a prepared product is stable in quality and convenient to store and meets quality requirements on the magnesium acetate tetrahydrate of the medicinal grade.

Description

technical field [0001] The invention belongs to the technical field of synthesis of chemical raw materials, in particular to a method for preparing medicinal magnesium acetate tetrahydrate. Background technique [0002] Magnesium acetate is a chemical raw material, used as a chemical reagent, a raw material for pharmaceuticals, and a catalyst for organic synthesis. In the field of medicine, magnesium acetate is used as an electrolyte in some injections, such as Pediatric Electrolyte Injection K1, Pediatric Electrolyte Injection K2, etc., all of which contain magnesium acetate in their prescriptions; therefore, this requires high-purity raw material pharmaceutical grade magnesium acetate raw material. [0003] At present, there are mainly the following methods for preparing magnesium acetate: (1) Magnesium acetate is produced by direct co-heating reaction of magnesium nitrate and acetic acid. The reaction process of this method is accompanied by the generation of nitric acid...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C51/42C07C51/43C07C53/10
CPCC07C51/412C07C51/42C07C51/43C07C53/10
Inventor 袁博邹凤仙冯新光
Owner HUAREN PHARMACEUTICAL CO LTD
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