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Process for preparing dexamethasone sodium phosphate by one-step method

A technology of dexamethasone sodium phosphate and step method, which is applied in the field of medicine, can solve the problems of long time, use of equipment and solvents, and cumbersome steps, and achieve the effects of simple method, reduced by-product generation, and high purity

Active Publication Date: 2020-12-18
西安国康瑞金制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The dexamethasone sodium phosphate product on the market at present, production technology must pass through this intermediate of dexamethasone phosphate, CN104744543A, CN101397320A, the synthesis technology research (week) of dissertation dexamethasone sodium phosphate all is to use dexamethasone Dexamethasone sodium phosphate is obtained through alkalization, acidification, and alkalization again to obtain fine dexamethasone sodium phosphate. The existing process has defects such as complicated steps, long time, and more equipment and solvents.

Method used

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  • Process for preparing dexamethasone sodium phosphate by one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 2000ml of anhydrous tetrahydrofuran into the reaction tank, add 392g (1.0mol) of dexamethasone, stir and disperse, cool down to -50°C, add 755g (3.0mol) of pyrophosphoryl chloride dropwise, keep the temperature constant, after the addition is complete After reacting for 1 hour, take a sample to detect that the residual dexamethasone is ≤1.0%, add 1000ml of purified water for hydrolysis, slowly warm up to room temperature, and fully stir. After the hydrolysis is completed, add 1500ml of toluene, let stand to separate the phases, collect the oil phase, add dropwise sodium hydroxide solution to the toluene oil phase to adjust the pH to 10, let stand to separate the phases, collect the water phase, add activated carbon to the water phase for decolorization for 30 minutes, Filtrate, pour all the liquid into the clean area, add acetone crystals equal to the volume of sodium hydroxide solution, grow the crystals, centrifuge, and dry to obtain 415g of dexamethasone sodium ph...

Embodiment 2

[0029] Add 2000ml of anhydrous tetrahydrofuran into the reaction tank, add 392g (1.0mol) of dexamethasone, stir and disperse, cool down to -50°C, add 1007g (4.0mol) of pyrophosphoryl chloride dropwise, keep the temperature constant, after the addition is complete After reacting for 1 hour, take a sample to detect that the residual dexamethasone is ≤1.0%, add 1000ml of purified water for hydrolysis, slowly warm up to room temperature, and fully stir. After the hydrolysis is completed, add 1500ml of toluene, let stand to separate the phases, collect the oil phase, add dropwise sodium hydroxide solution to the toluene oil phase to adjust the pH to 10, let stand to separate the phases, collect the water phase, add activated carbon to the water phase for decolorization for 30 minutes, Filtrate, pour all the liquid into the clean area, add acetone crystals equal to the volume of sodium hydroxide solution, grow the crystals, centrifuge, and dry to obtain 445g of dexamethasone sodium p...

Embodiment 3

[0031] Add 2000ml of anhydrous tetrahydrofuran into the reaction tank, add 392g (1.0mol) of dexamethasone, stir and disperse, cool down to -50°C, add 1259g (5.0mol) of pyrophosphoryl chloride dropwise, keep the temperature constant, after the addition is complete After reacting for 1 hour, take a sample to detect that the residual dexamethasone is ≤1.0%, add 1000ml of purified water for hydrolysis, slowly warm up to room temperature, and fully stir. After the hydrolysis is completed, add 1500ml of toluene, let stand to separate the phases, collect the oil phase, add dropwise sodium hydroxide solution to the toluene oil phase to adjust the pH to 10, let stand to separate the phases, collect the water phase, add activated carbon to the water phase for decolorization for 30 minutes, Filtrate, pour all the liquid into the clean area, add acetone crystals equal to the volume of sodium hydroxide solution, grow the crystals, centrifuge, and dry to obtain 482g of dexamethasone sodium p...

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Abstract

The invention provides a process for producing dexamethasone sodium phosphate by a one-step method, which comprises the following steps of by using dexamethasone as a starting raw material, carrying out (1) pyrophosphoryl chloride esterification, (2) purified water hydrolysis, (3) toluene extraction purification, sodium hydroxide alkalization treatment, (4) activated carbon decolorization and (5)acetone crystallization to obtain the high-purity dexamethasone sodium phosphate product at high yield. The product obtained by the process is stable in quality, the use of equipment and solvents is reduced, the method is simple and convenient, the production cost is greatly reduced, and the process is more suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a preparation process for producing dexamethasone sodium phosphate in one step. Background technique [0002] Dexamethasone sodium phosphate is also called dexamethasone sodium phosphate, its chemical name is 1,4-pregna-9α-fluoro-16α-methyl-11β,17α,21-triol-3,20-dione-21- Phosphate disodium salt belongs to adrenal cortex hormone drugs and is widely used in anti-inflammatory, anti-allergic, anti-rheumatic, immunosuppressive and other fields. [0003] The dexamethasone sodium phosphate product on the market at present, production technology must pass through this intermediate of dexamethasone phosphate, CN104744543A, CN101397320A, the synthesis technology research (week) of dissertation dexamethasone sodium phosphate all is to use dexamethasone The phosphoric acid ester is alkalized, acidified, and alkalized again to obtain the high-quality dexamethasone sodium phosphate. The exi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J51/00
CPCC07J51/00
Inventor 王培文刘伟李娜蒲飞飞张恒
Owner 西安国康瑞金制药有限公司
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