Dexamethasone sodium phosphate crystal form and its crystallization preparation method

A technology of dexamethasone sodium phosphate and crystal form, which is applied in the field of crystal form and crystallization preparation of dexamethasone sodium phosphate, can solve the problems affecting product purity, storage time, heat resistance, etc., and achieve high crystallinity, Easy to filter, good thermal stability

Active Publication Date: 2006-04-26
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the difference in crystal form has no effect on the efficacy of the drug, it will have a large dif

Method used

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  • Dexamethasone sodium phosphate crystal form and its crystallization preparation method
  • Dexamethasone sodium phosphate crystal form and its crystallization preparation method
  • Dexamethasone sodium phosphate crystal form and its crystallization preparation method

Examples

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Example Embodiment

[0027] Example 1

[0028] Add 120g of dexamethasone phosphate into a three-necked flask, add 2000ml of ethanol and 6g of activated carbon at the same time, stir and dissolve at a constant temperature of 40°C, and filter after continuous stirring for 60 minutes. The filtrate is moved in the crystallizer, and configuration concentration is the sodium hydroxide solution of 100g / L simultaneously. Then sodium hydroxide solution is added into the crystallizer for reaction, and the pH value at the end of the reaction process is controlled at 11.0. Add about 4000 ml of diethyl ether-water mixed solvent to the reacted dexamethasone sodium phosphate solution while stirring at 20° C. to crystallize. After the crystallization is finished, carry out centrifugation, wash with acetone, and dry the obtained crystal product at 70° C. and a pressure of 0.1 MPa for 6 hours, and then dry at this temperature for 15 hours at a pressure of 0.008 MPa. The content of the final crystal product is 99....

Example Embodiment

[0029] Example 2

[0030] Add 12g of dexamethasone phosphate into a three-necked flask, add 120ml of ethanol and 1.2g of activated carbon at the same time, stir and dissolve at a constant temperature of 40°C, and filter after continuous stirring for 30 minutes. The filtrate is moved in the crystallizer, and configuration concentration is the sodium hydroxide solution of 100g / L simultaneously. Then sodium hydroxide solution is added into the crystallizer for reaction, and the pH value at the end of the reaction process is controlled at 10.5. Add about 360 ml of diethyl ether-water mixed solvent to the reacted dexamethasone sodium phosphate solution while stirring at 25° C. for crystallization. Centrifuge after crystallization, wash with ethanol, dry the obtained crystal product at 50° C. and a pressure of 0.1 MPa for 6 hours, and then dry at this temperature for 14 hours at 0.002 MPa. The content of the final crystal product is 99.3%, and the quality conforms to the latest ph...

Example Embodiment

[0031] Example 3

[0032] Add 6g of dexamethasone phosphate into a three-necked flask, add 50ml of methanol and 0.5g of activated carbon at the same time, stir and dissolve at a constant temperature of 45°C, and filter after continuous stirring for 60 minutes. The filtrate is moved into the crystallizer, and the sodium hydroxide solution of 250g / L is configured simultaneously. Then sodium hydroxide solution is added into the crystallizer for reaction, and the pH value at the end of the reaction process is controlled at 9.5. Add about 300 ml of ethanol-water mixed solvent to the reacted dexamethasone sodium phosphate solution while stirring at 20° C. to crystallize. After the crystallization is completed, carry out centrifugation, wash with ethanol, and dry the obtained crystal product at a temperature of 80° C. and a pressure of 0.1 MPa for 5 hours, and then at this temperature of 0.009 MPa for 10 hours. The content of the final crystal product is 99.4%, and the quality conf...

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Abstract

The present invention is dexamethasone sodium phosphate crystal and its preparation process. The preparation process includes the following steps: mixing dexamethasone phosphate, alcohol solvent and active carbon in certain proportion in a reactor at 35-45 deg.c via stirring for 30-60 min, and filtering; transferring the filtrate into crystallizer, adding 100-250 g/L sodium hydroxide solution to react at constant temperature in 15-35 deg.c and controlling reaction terminal pH 9-12.5; adding separating agent in the amount of 2-6 times the solvent volume to crystallize after reaction; and centrifugal separating and drying at 40-80 deg.c and 0.002-0.1 MPa for 15-24 hr. Thus prepared crystal belongs to Pmc21 space group of orthorhombic system. The process has high crystal product quality and yield.

Description

technical field [0001] The invention belongs to the technical field of crystallization, and in particular relates to a crystal form of dexamethasone sodium phosphate and a crystallization preparation method thereof. Background technique [0002] The chemical name of dexamethasone sodium phosphate is 16α-methyl-11β,17α,21-trihydroxy-9α-fluoropregna-1,4-diene-3,20-dione-21- Phosphate disodium salt, molecular formula C 22 h 28 FO 8 PNa 2 , the molecular weight is 516.4, and its chemical structure is as follows figure 1 shown. [0003] Dexamethasone Sodium Phosphate is a kind of adrenal glucocorticoid drugs. It has stronger anti-inflammatory, anti-toxin and anti-shock effects, and has no sodium retention and potassium excretion effects. It is indispensable for rescuing critically ill patients. Emergency medicine, once known as the "king of corticosteroid drugs" in the 1970s. Its raw materials can be made into clinical injection injections, ...

Claims

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Application Information

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IPC IPC(8): C07J7/00B01D9/00
Inventor 王静康王福军王永莉张美景郝红勋
Owner TIANJIN UNIV
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