Sodium fusidate crystallization method

A technology of sodium fusidate and crystallization, applied in the directions of steroids, organic chemistry, etc., can solve the problems of poor stability of sodium fusidate crystals, unfavorable preservation and sub-packaging, and high production costs, and achieves a crystal clear appearance, The effect of uniform particles and good fluidity

Active Publication Date: 2013-04-03
NCPC NEW DRUG RES & DEV
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Problems solved by technology

Though this method has improved the purity of sodium fusidate crystal to a certain extent, has improved crystal outward appearance, still has many weak points, for example this method adopts mul

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  • Sodium fusidate crystallization method

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Embodiment 1

[0018] Example 1 Preparation of high-quality sodium fusidate crystals by sodium fusidate solid

[0019] a. Weigh 7 g of sodium fusidate solid, and dissolve it in an aqueous solution of acetone with an acetone concentration of 80% (by volume ratio) at room temperature, and stir for 0.5-3 hours to obtain 21 mL of sodium fusidate solution;

[0020] b. Heat the above-mentioned sodium fusidate solution to 40°C and keep it warm, add acetone while stirring, and the flow rate is 20mL / h. The acceleration rate is reduced to 10mL / h. When the feeding amount of acetone is 210mL, stop feeding and let stand for 18h (crystal growth); after standing, filter and separate solid and liquid;

[0021] c. The filter cake was rinsed with acetone and dried at 40-45°C for 24 hours to obtain 6.5 g of sodium fusidate crystals, which were determined by HPLC with a purity of 99.8% and a yield of 93.2%. The obtained sodium fusidate crystal has a stable crystal form and good fluidity (measured value of spec...

Embodiment 2

[0022] Example 2 Preparation of high-quality sodium fusidate crystals from fusidic acid solids

[0023] a. Weigh 7g of fusidic acid solid, and at normal temperature, dissolve it in an aqueous solution of 50% acetone with acetone volume ratio concentration, stir until dissolved, add dropwise 4M aqueous sodium hydroxide solution under stirring, the added hydrogen The mol ratio of sodium oxide and fusidic acid is 0.8:1, obtains sodium fusidic acid solution 25mL;

[0024] b. Heat the above-mentioned sodium fusidate solution to 30°C and keep it warm, add acetone while stirring, and the flow rate is 22mL / h. When the sodium fusidate solution becomes turbid, reduce the flow rate to 6mL / h h, when the feeding amount of acetone is 250mL, stop feeding and let stand for 16h;

[0025] c. After standing still, filter with suction, rinse the filter cake with acetone and dry it at 40-42°C for 20 hours to obtain 6.3g of sodium fusidate crystals. The purity is 99.8% and the yield is determined ...

Embodiment 3

[0026] Example 3 Preparation of high-quality sodium fusidate crystals from fusidic acid solids

[0027] a. Weigh 7g of fusidic acid solid, and at normal temperature, dissolve it in an aqueous solution of acetone with acetone volume ratio concentration of 90%, stir until dissolved, then add dropwise 4M aqueous sodium hydroxide solution under stirring, and the The mol ratio of sodium oxide and fusidic acid is 1.2:1, obtains sodium fusidic acid solution 30mL;

[0028] b. Heat the above-mentioned sodium fusidate solution to 60°C and keep it warm, add acetone while stirring, and the flow acceleration rate is 24mL / h. When the sodium fusidate solution becomes turbid, reduce the flow acceleration rate to 18mL / h h, when the feeding amount of acetone is 450mL, stop feeding and let stand for 20h;

[0029] c. After standing still, filter with suction, rinse the filter cake with acetone and dry it at 44-45°C for 40h to obtain 6.6g of sodium fusidate crystals. The purity is 99.7% and the y...

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Abstract

The invention provides a sodium fusidate crystallization method which comprises the following steps: a, preparing a sodium fusidate solution by taking a acetone water solution as solvent; b, heating the sodium fusidate solution, feeding acetone while stirring, reducing the feeding rate when the sodium fusidate solution is turbid, and standing for crystallization after the feeding operation is finished; and performing solid-liquid separation, leaching the obtained solids with acetone, and then drying to obtain sodium fusidate crystals. According to the invention, the method is simple to operate and low in cost; and the sodium fusidate crystals prepared by the method are stable in crystal form and favorable in flowability.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, in particular to a crystallization method of sodium fusidate. Background technique [0002] Fusidic acid is a fusidic acid antibiotic produced by the fermentation of lipococcus fusidi, which is sensitive to Gram-positive bacteria, and its sodium salt is commonly used clinically. Fusidate sodium (Fusidate Sodium) can be prepared by the reaction of fusidic acid and sodium hydroxide. The molecular formula of sodium fusidate is C 31 h 47 NaO 6 , the molecular weight is 538.70, and its structure is shown in formula (1): [0003] [0004] At present, the industrial method for preparing high-quality sodium fusidate crystals usually involves crystallizing a solution containing sodium fusidate with various organic solvents. Though this method has improved the purity of sodium fusidate crystal to a certain extent, has improved crystal outward appearance, still has many weak points, for ex...

Claims

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Application Information

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IPC IPC(8): C07J13/00
Inventor 仲伟潭郭月玲李敏娜王崔岩张雪霞朱秀良董爱华任志红宋霏
Owner NCPC NEW DRUG RES & DEV
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