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Preparation method of amcinonide

An amcinonide and reaction technology, which is applied to the preparation field of amcinonide, can solve the problems of low yield of amcinonide, expensive raw materials and high production cost, and achieves the effects of easy production scale-up, cost reduction and good quality.

Active Publication Date: 2021-11-26
SHANDONG GUYUCHUN BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Starting from 9α-fluoro-11β,16α,17α,21-tetrahydroxypregnenoic acid-1,4-diene-3,20-dione, it was ketalized by the reaction of perchloric acid and cyclopentanone, and then Acetic anhydride is added to pyridine to obtain amcinonide. The raw materials used in this method are expensive, and the yield of amcinonide obtained is low (about 50%) and poor in quality, resulting in high production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation method of amcinonide, its reaction route is:

[0029] .

[0030] The specific steps are:

[0031] (1) Add hydrofluoric acid and acetone into the reactor, stir to cool down to -30°C, add compound I (10g) in batches, and keep it at -30°C for 3 hours; after the reaction is completed, slowly raise the temperature to 0°C and add cyclopentanone dropwise , after dropping, keep warm at 0°C for 3 hours; after the reaction, add the reaction solution dropwise to ice water, adjust the pH to neutral, stir, crystallize, filter, rinse the filter cake with water, and dry to obtain intermediate II. 92.4%, purity 96.3%;

[0032] (2) Add intermediate II (10g) to the reactor, add acetone, add potassium carbonate while stirring at 20°C, add acetic anhydride dropwise, after the addition is complete, stir at 20°C for 5 hours, and when the reaction is complete, add the reaction solution to In ice water, stirred, crystallized, filtered, and dried to obtain the crude p...

Embodiment 2

[0046] A method for preparing amcinonide, the reaction scheme of which is the same as in Example 1.

[0047] The specific steps are:

[0048] (1) Add hydrofluoric acid and acetone to the reactor, stir and cool down to -25°C, add compound I (10g) in batches, and keep it at -25°C for 4 hours; after the reaction is completed, slowly raise the temperature to 5°C and add cyclopentanone dropwise , after dropping, keep warm at 10°C for 3 hours; after the reaction, add the reaction solution dropwise to ice water, adjust the pH to neutral, stir, crystallize, filter, rinse the filter cake with water, and dry to obtain intermediate II. 91.8%, purity 96.7%;

[0049] (2) Add intermediate II (10g) to the reactor, add acetone, add potassium carbonate while stirring at 20°C, add acetic anhydride dropwise, after the addition is complete, stir at 20°C for 5 hours, and when the reaction is complete, add the reaction solution to In ice water, stirred, crystallized, filtered, and dried to obtain...

Embodiment 3

[0063] A method for preparing amcinonide, the reaction scheme of which is the same as in Example 1.

[0064] The specific steps are:

[0065] (1) Add hydrofluoric acid and acetone into the reactor, stir and cool down to -30°C, add compound I (10g) in batches, and keep it at -30°C for 3 hours; after the reaction is completed, slowly raise the temperature to 5°C and add cyclopentanone dropwise , after dropping, keep warm at 10°C for 2 hours; after the reaction, add the reaction solution dropwise to ice water, adjust the pH to neutral, stir, crystallize, filter, rinse the filter cake with water, and dry to obtain intermediate II. 92.1%, purity 96.5%;

[0066] (2) Add intermediate II (10g) to the reactor, add acetone, add potassium carbonate while stirring at 30°C, add acetic anhydride dropwise, after the addition is complete, stir and react at 30°C for 3h, after the reaction is complete, add the reaction solution to In ice water, stirred, crystallized, filtered, and dried to obta...

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PUM

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Abstract

The invention belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of amcinonide. The method comprises steps: taking a compound I as a raw material, firstly reacting with hydrofluoric acid and cyclopentanone, and then reacting under the action of acetic anhydride and potassium carbonate to obtain the amcinonide. Compared with the prior art, the compound I with lower price is used as a production raw material, so that the cost is reduced, the production amcinonide is easier, the yield is increased, and the amcinonide with better quality is obtained.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of amcinonide. Background technique [0002] Amcinonide is a topical corticosteroid used primarily as an anti-inflammatory and antipruritic agent to reduce or inhibit the action of chemicals in the body that cause inflammation, redness, and swelling. When given in ointment, Amcinonide also helps Keeps moisture in the skin. Its chemical structural formula is: [0003] . [0004] In the prior art, the synthetic route of amcinonide is: [0005] . [0006] Starting from 9α-fluoro-11β,16α,17α,21-tetrahydroxypregnenoic acid-1,4-diene-3,20-dione, it was ketalized by the reaction of perchloric acid and cyclopentanone, and then Adding acetic anhydride to pyridine to obtain amcinonide, the raw materials used in this method are expensive, the yield of amcinonide obtained is low (about 50%), and the quality is poor, resulting in high produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
CPCC07J71/0031
Inventor 杨凯袁文博王春燕王文静靳安琪
Owner SHANDONG GUYUCHUN BIOTECHNOLOGY CO LTD
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