Preparing method of cortisone acetate

A technology of cortisone acetate and iodine solution, applied in the field of chemistry, can solve the problems of easy sublimation of iodine monoplex, large environmental pollution and high cost, and achieve the effects of low cost, reduced environmental pollution and reduced iodine consumption

Active Publication Date: 2016-06-15
河北远大九孚生物科技有限公司
View PDF4 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of iodination reaction, due to the easy sublimation of iodine, the consumption is large, the cost is high, and the pollution to the environment is large.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparing method of cortisone acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step 1, the preparation of bromine-iodine solution

[0021] Put 200L of methanol and 19.5kg of anhydrous calcium chloride into the bromine-iodine solution preparation tank. When the temperature is less than 25°C, put 57.5kg of iodine solution into the preparation tank and stir for more than 1.0 hours; vacuum pulls in 33.4kg of bromine, After continuing to stir and fully dissolve, pull in the bromine-iodine solution and add it dropwise to the high-level tank, and set aside;

[0022] Step 2, iodination reaction

[0023] Add 19.5kg calcium chloride and 200L methanol in the reaction device, add 650L chloroform, 130kg reactant 17α-hydroxyl-pregn-4-ene-3,11,20-trione (I) after dissolving, control temperature is 10 At about ℃, add 75kg of calcium oxide, continue to cool down to below -3 ℃, slowly add bromine iodine solution, control the temperature not higher than 0 ℃, first slowly and then quickly, about 1-1.5h to finish the drop, after the drop is over -3 Incubate at ~0°C ...

Embodiment 2

[0027] Step 1, the preparation of bromine-iodine solution

[0028] Put 200L of methanol and 19.5kg of anhydrous zinc chloride into the bromine-iodine solution preparation tank. When the temperature is less than 25°C, put 57.5kg of iodine solution into the preparation tank and stir for more than 1.0 hours; vacuum pulls in 33.4kg of bromine , continue to stir and fully dissolve, pull in the bromine-iodine solution and add it dropwise to the high-level tank, and set aside;

[0029] Step 2, iodination reaction

[0030] Add 19.5kg zinc chloride and 200L methanol in the reaction device, add dichloromethane, 130kg reactant 17α-hydroxyl-pregna-4-ene-3,11,20-triketone (I) after dissolving, control temperature is At about 10°C, add 75kg of zinc oxide, continue to cool down to below -3°C, slowly add bromine-iodine solution, control the temperature not higher than 0°C, first slowly and then quickly, about 1-1.5h to finish dripping, after dripping - Incubate at 3-0°C for 3-3.5h, after th...

Embodiment 3

[0034] The reaction steps and conditions are basically the same as in Example 1, except that zinc chloride is used in steps 1 and 2 to replace calcium chloride as a cosolvent.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a preparing method of cortisone acetate. The method comprises the three following steps of iodine solution preparation, the iodo reaction and the replacement reaction. In the step one, an idodine solution and bromine are mixed to prepare bromine and iodine liquid. In the step two of the iodo reaction, a reactant 17 alpha-hydroxyl-pregnene-4-alkene-3,11,20-triketone (I) and the bromine and iodine liquid are subjected to the iodo reaction to obtain an intermediate product iodine substitute (II). In the step three of the replacement reaction, the iodine substitute (II) and acetate are subjected to the replacement reaction to obtain a final product cortisone acetate (III). According to the preparing method, the bromine and iodine mixture iodo reaction replaces the traditional iodo reaction, the amount of adopted iodine is reduced greatly, cost is low, environmental pollution is reduced, and applicability is high.

Description

technical field [0001] The invention relates to a preparation method of cortisone acetate, which belongs to the field of chemistry. Background technique [0002] Cortisone acetate is used for anti-inflammation due to its strong anti-inflammatory effect. Mainly used for the replacement therapy of adrenal insufficiency. The dosage forms listed in the 1990s mainly include suspension (for local injection) and cortisone acetate tablet. Due to its relatively large side effects, it has been replaced by drugs such as hydrocortisone. And cortisone acetate itself is used as an intermediate of steroid medicines to produce raw materials such as hydrocortisone and prednisolone. [0003] At present, the process of synthesizing cortisone acetate in China is mainly the diene route successfully developed by Huang Minglong, the father of Chinese steroid chemistry in 1958, or the route modified with AD as the substrate to obtain debrominated products, and then debrominated Cortisone acetat...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
CPCC07J5/0053
Inventor 李超余伟
Owner 河北远大九孚生物科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap