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Preparation technology for dexamethasone sodium phosphate

A technology for preparing dexamethasone sodium phosphate, which is applied in the field of medicine, can solve the problems of complex process and low yield, and achieve the effect of easy-to-obtain raw materials, low cost and simple steps

Inactive Publication Date: 2016-02-24
CHINA CHENGDU ANIMAL HUSBANDRY IND BIOPHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation method of existing dexamethasone sodium phosphate has complicated process and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation process of dexamethasone sodium phosphate, comprising the following steps:

[0022] 1) Ring-opening reaction: use dexamethasone acetate epoxy as the starting material, add HF and DMF, the reaction temperature is -10°C, and the reaction time is 3 hours for ring-opening reaction to obtain dexamethasone acetate solution, dexamethasone acetate The molar ratio of epoxy, HF, DMF is 1:92:44;

[0023] 2) Recrystallization: add acetone to the dexamethasone acetate solution for recrystallization to obtain dexamethasone acetate, and remove the solvent by rotary evaporation after recrystallization;

[0024] 3), base-catalyzed hydrolysis: adding the dexamethasone acetate obtained in step 2) to Na 2 CO 3 and methanol, the reaction temperature is 20°C, and the reaction time is 10 minutes to obtain dexamethasone, dexamethasone acetate, Na 2 CO 3 , The molar ratio of methanol is 1:4:214;

[0025] 4) Esterification of pyrophosphoryl chloride: react the dexamethasone ob...

Embodiment 2

[0028] A preparation process of dexamethasone sodium phosphate, comprising the following steps:

[0029] 1) Ring-opening reaction: use dexamethasone acetate epoxy as the starting material, add HF and DMF, the reaction temperature is -5°C, and the reaction time is 3 hours for ring-opening reaction to obtain dexamethasone acetate solution, dexamethasone acetate The molar ratio of epoxy, HF, DMF is 1.5:94:48;

[0030] 2) Recrystallization: add acetone to the dexamethasone acetate solution for recrystallization to obtain dexamethasone acetate, and remove the solvent by rotary evaporation after recrystallization;

[0031] 3), base-catalyzed hydrolysis: adding the dexamethasone acetate obtained in step 2) to Na 2 CO 3 and methanol, the reaction temperature is 25°C, and the reaction time is 10 minutes to obtain dexamethasone, dexamethasone acetate, Na 2 CO 3 , the mol ratio of methyl alcohol is 1.5:6:216;

[0032] 4) Esterification of pyrophosphoryl chloride: react the dexametha...

Embodiment 3

[0035] A preparation process of dexamethasone sodium phosphate, comprising the following steps:

[0036] 1) Ring-opening reaction: use dexamethasone acetate epoxy as the starting material, add HF and DMF, the reaction temperature is 0°C, and the reaction time is 3 hours to carry out the ring-opening reaction to obtain the dexamethasone acetate solution, and the dexamethasone acetate ring The molar ratio of oxygen, HF, and DMF is 2:95:50;

[0037] 2) Recrystallization: add ether to the dexamethasone acetate solution for recrystallization to obtain dexamethasone acetate, and remove the solvent by rotary evaporation after recrystallization;

[0038] 3), base-catalyzed hydrolysis: adding the dexamethasone acetate obtained in step 2) to Na 2 CO 3 and methanol, the reaction temperature is 30°C, and the reaction time is 10 minutes to obtain dexamethasone, dexamethasone acetate, Na 2 CO 3 , the mol ratio of methyl alcohol is 2:8:220;

[0039] 4) Esterification of pyrophosphoryl c...

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PUM

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Abstract

The invention relates to a preparation technology for dexamethasone sodium phosphate. The preparation technology comprises the following steps: a ring-opening reaction is carried out, namely, dexamethasone acetate epoxide is employed as an initial raw material, HF and DMF are added, a reaction is performed for 3h, a ring-opening reaction is carried out and a dexamethasone acetate solution is prepared; recrystallization is carried out, namely, acetone or ether is added in the dexamethasone acetate solution, recrystallization is carried out, dexamethasone acetate is prepared, and rotary distillation is employed to remove the solvent after recrystallization; base catalysis hydrolysis is carried out, namely, dexamethasone acetate is added in Na2CO3 and methanol, a reaction is carried out for 10min, dexamethasone is prepared; pyrophosphoryl chlorine esterification is carried out, namely, dexamethasone is reacted with pyrophosphoryl chlorine and THF, and dexamethasone phosphate ester is prepared; a neutralization salt forming reaction is carried out, namely, the dexamethasone phosphate ester obtained from the fourth step is reacted with NaOH and methanol, and dexamethasone sodium phosphate is prepared. The steps are simple, raw materials are easily available, the reaction conditions are mild, the preparation technology is suitable for industrial production, and the cost is low.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a preparation process of dexamethasone sodium phosphate. Background technique [0002] Dexamethasone sodium phosphate, chemical name 16α-methyl-11β,17α,21 trihydroxy-9α-flupregna-1,4-diene-3,20-dione-21-phosphate disodium salt, It is an adrenocortical hormone drug with anti-inflammatory, anti-allergic, anti-rheumatic and immunosuppressive effects. The mechanism of action is: (1) Anti-inflammatory effect: it can reduce and prevent the response of tissues to inflammation, thereby reducing the manifestation of inflammation. It can inhibit the accumulation of inflammatory cells, including macrophages and leukocytes at the site of inflammation, and inhibit phagocytosis, the release of lysosomes, and the synthesis and release of inflammatory chemical mediators. (2) Immunosuppressive effect: including preventing or inhibiting cell-mediated immune response, delayed allergic reaction, ...

Claims

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Application Information

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IPC IPC(8): C07J51/00
Inventor 廖成斌卢朝成
Owner CHINA CHENGDU ANIMAL HUSBANDRY IND BIOPHARM
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