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Synthetic method for pregnatriene-16alpha-methyl-17alpha,21-diol-3,20-dione-21-acetate

A synthetic method and acetate technology, applied in the direction of steroids, organic chemistry, etc., can solve the problems of high heat resistance requirements for reaction equipment, increased manufacturing costs, and reduced reaction costs, so as to avoid the risk of poisoning and reduce the intermediate links of the reaction , the effect of reducing the reaction cost

Inactive Publication Date: 2018-07-03
CHENGDU KA DI FU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, the reaction temperature required for this synthesis method needs to be maintained above 110°C for as long as 14 hours, which will lead to higher requirements for heat resistance of the reaction equipment, increased equipment maintenance and manufacturing costs, and the maintenance of high temperature conditions. Energy consumption is higher, is unfavorable for reducing reaction cost, therefore, there are many shortcomings in above-mentioned synthetic method, be necessary to propose a kind of new synthetic method

Method used

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  • Synthetic method for pregnatriene-16alpha-methyl-17alpha,21-diol-3,20-dione-21-acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The synthetic method of pharmaceutical intermediate 1,4,9(11)-pregnatriene-16α-methyl-17α,21-diol-3,20-diketone-21-acetate comprises the following steps:

[0017] A: Add 3mol 2-hydroxyl-4,9(11)-pregnadiene-16α-methyl-17α,21-diol-3,20-diketone-21-acetate in the reaction vessel, 900ml quality For a propionitrile solution with a fraction of 30%, raise the temperature of the solution to 50°C, add 3 mol of potassium peroxodisulfate, 1.2L of an oxalic acid solution with a mass fraction of 20%, and react for 40 minutes;

[0018] B: Raise the temperature of the solution to 60°C, add 3mol of chloroauric acid powder, 800ml of sodium sulfate solution with a mass fraction of 15%, continue the reaction for 2h, adjust the pH to 6, let it stand for 30min, and use 10% of the mass fraction to chlorinate Wash 3 times with sodium solution, wash 2 times with 70% ethylbenzene solution, recrystallize in 85% ethylene glycol dimethyl ether solution, dehydrate with dehydrating agent anhydrous m...

Embodiment 2

[0020] The synthetic method of pharmaceutical intermediate 1,4,9(11)-pregnatriene-16α-methyl-17α,21-diol-3,20-diketone-21-acetate comprises the following steps:

[0021] A: Add 3mol 2-hydroxyl-4,9(11)-pregnadiene-16α-methyl-17α,21-diol-3,20-diketone-21-acetate in the reaction vessel, 900ml quality For a propionitrile solution with a fraction of 33.5%, raise the solution temperature to 53.5°C, add 3.5mol potassium peroxodisulfate, 1.2L oxalic acid solution with a mass fraction of 23%, and react for 50 minutes;

[0022] B: raise the temperature of the solution to 63°C, add 3.5mol of chloroauric acid powder, 800ml of sodium sulfate solution with a mass fraction of 18.5%, continue the reaction for 2.5h, adjust the pH to 6.25, let stand for 40min, and use a mass fraction of 12.5% Wash 4 times with sodium chloride solution, wash 3 times with 73% ethylbenzene solution, recrystallize in 88.5% ethylene glycol dimethyl ether solution, dehydrate with dehydrating agent anhydrous magnesium...

Embodiment 3

[0024] The synthetic method of pharmaceutical intermediate 1,4,9(11)-pregnatriene-16α-methyl-17α,21-diol-3,20-diketone-21-acetate comprises the following steps:

[0025] A: Add 3mol 2-hydroxyl-4,9(11)-pregnadiene-16α-methyl-17α,21-diol-3,20-diketone-21-acetate in the reaction vessel, 900ml quality For a propionitrile solution with a fraction of 37%, raise the temperature of the solution to 57°C, add 4 mol of potassium peroxodisulfate, 1.2L of an oxalic acid solution with a mass fraction of 26%, and react for 60 minutes;

[0026] B: Raise the temperature of the solution to 66°C, add 4mol of chloroauric acid powder, 800ml of sodium sulfate solution with a mass fraction of 22%, continue the reaction for 3h, adjust the pH to 6.5, let it stand for 50min, and use 15% of the mass fraction to chlorinate Wash 5 times with sodium solution, wash 4 times with ethylbenzene solution with mass fraction of 76%, recrystallize in ethylene glycol dimethyl ether solution with mass fraction of 92%...

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Abstract

The invention discloses a synthetic method for the drug intermediate 1,4,9(11)-pregnatriene-16alpha-methyl-17alpha,21-diol-3,20-dione-21-acetate. The synthetic method comprises the following steps: adding 2-hydroxy-4,9(11)-pregnadiene-16beta-methyl-17alpha,21-diol-3,20-dione-21-acetate and a propionitrile solution into a reaction vessel, raising a solution temperature, adding potassium peroxydisulfate and carrying out a reaction; and raising the solution temperature, adding chloroauric acid powder and a sodium sulfate solution, continuing the reaction, adjusting a pH value, carrying out standing, then carrying out washing with a sodium chloride solution a plurality of times, then carrying out washing with an ethylbenzene solution a plurality of times, then carrying out recrystallization inan ethylene glycol dimethyl ether solution, and carrying out dehydration with a dehydrating agent to obtain the finished 1,4,9(11)-pregnatriene-16alpha-methyl-17alpha,21-diol-3,20-dione-21-acetate.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, belonging to the field of organic synthesis, in particular to a pharmaceutical intermediate 1,4,9(11)-pregnatriene-16α-methyl-17α,21-diol-3, Synthesis of 20-diketone-21-acetate. Background technique [0002] 1,4,9(11)-pregnatriene-16α-methyl-17α,21-diol-3,20-diketone-21-acetate is mainly used Dexamethasone acetate, dexamethasone acetate is an adrenal corticosteroid and adrenocorticotropic hormone drug, which can be used to resist various inflammations and allergic reactions of skin and mucous membranes; eye ointment can be used to treat various ophthalmia. Most of the existing synthetic methods use defatted matter, butyl acetate, selenium dioxide, methanol and other raw materials as reactants, the reaction temperature is above 110°C, and the maintenance time is above 14 hours. However, the raw material selenium dioxide used in this synthesis method is a highly toxic subst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
CPCC07J5/0076
Inventor 廖如佴
Owner CHENGDU KA DI FU TECH
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