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A kind of preparation method of high-purity fluocinolone

A technology of fluocinolone and water purification, applied in the fields of steroids, organic chemistry, etc.

Active Publication Date: 2020-04-28
ZHEJIANG REACHALL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is currently no production of fluocinolone that meets the medicinal requirements in China

Method used

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  • A kind of preparation method of high-purity fluocinolone
  • A kind of preparation method of high-purity fluocinolone
  • A kind of preparation method of high-purity fluocinolone

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preparation example Construction

[0028] In order to solve the above-mentioned technical problems, the invention provides a kind of preparation method of high-purity fluocinolone, the preparation method of described high-purity fluocinolone comprises the following steps:

[0029] (1) Add 11β-hydroxyl-16α,17-[(1-methylethylene)-bis(oxygen)]-21-(acetyloxy)-6α,9-difluoropregna- 1,4-diene-3,20-dione, the first organic solvent, pass in an inert gas, stir; cool down to 0-5°C, add a hydrolysis reagent, keep warm for 4-10 hours, adjust the pH with acetic acid after the reaction When the value reaches 6-7, heat up to 35-45°C, concentrate under reduced pressure to 10-35% of the weight of the solution before concentration, add purified water dropwise, and keep stirring at 5-15°C for 1-3h; filter and use the mass fraction Rinse with 30-70% ethanol, and dry under reduced pressure at 60°C to obtain 11β, 21-dihydroxy-16α,17-[(1-methylethylene)-bis(oxygen)]-6α,9- Crude difluoropregna-1,4-diene-3,20-dione;

[0030](2) Add 11...

Embodiment 1

[0084] The preparation method of described high-purity fluocinolone comprises the following steps:

[0085] (1) Add 11β-hydroxyl-16α,17-[(1-methylethylene)-bis(oxygen)]-21-(acetyloxy)-6α,9-difluoropregna- 1,4-diene-3,20-dione, the first organic solvent, pass inert gas, stir; cool down to 2°C, add hydrolysis reagent, keep warm for 6 hours, after the reaction, adjust the pH value to 6- 7. Heat up to 40°C, concentrate under reduced pressure to 30% of the weight of the solution before concentration, add purified water dropwise, and keep stirring at 10°C for 2 hours; filter, rinse with ethanol with a mass fraction of 50%, and reduce Press and dry to get 11β, 21-dihydroxy-16α, 17-[(1-methylethylene)-bis(oxygen)]-6α, 9-difluoropregna-1,4-diene-3, 20-diketone crude product; the first organic solvent is absolute ethanol; the inert gas is nitrogen; the 11β-hydroxyl-16α, 17-[(1-methylethylene)-bis(oxygen)] The weight ratio of -21-(acetyloxy)-6α,9-difluoropregna-1,4-diene-3,20-dione to ...

Embodiment 2

[0089] The preparation method of described high-purity fluocinolone comprises the following steps:

[0090] (1) Add 11β-hydroxyl-16α,17-[(1-methylethylene)-bis(oxygen)]-21-(acetyloxy)-6α,9-difluoropregna- 1,4-diene-3,20-dione, the first organic solvent, pass inert gas, stir; cool down to 2°C, add hydrolysis reagent, keep warm for 6 hours, after the reaction, adjust the pH value to 6- 7. Heat up to 40°C, concentrate under reduced pressure to 30% of the weight of the solution before concentration, add purified water dropwise, and keep stirring at 10°C for 2 hours; filter, rinse with ethanol with a mass fraction of 50%, and reduce Press and dry to get 11β, 21-dihydroxy-16α, 17-[(1-methylethylene)-bis(oxygen)]-6α, 9-difluoropregna-1,4-diene-3, 20-diketone crude product; the first organic solvent is absolute ethanol; the inert gas is nitrogen; the 11β-hydroxyl-16α, 17-[(1-methylethylene)-bis(oxygen)] The weight ratio of -21-(acetyloxy)-6α,9-difluoropregna-1,4-diene-3,20-dione to ...

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Abstract

The invention provides a preparation method of high-purity fluocinolone acetonide. The preparation method comprises the following steps: (1) performing hydrolysis reaction on 11 beta-hydroxyl-16 alpha,17-[(1-methyl ethylidene)-bis (oxygen)]-21-(acetoxy)-6 alpha,9-difluorobenzene-1,4-diene-3,20-diketone; (2) refining a 11 beta-hydroxyl-16 alpha,17-[(1-methyl ethylidene)-bis (oxygen)]-6 alpha,9-difluorobenzene-1,4-diene-3,20-diketone crude product to obtain a 11 beta-hydroxyl-16 alpha,17-[(1-methyl ethylidene)-bis (oxygen)]-6 alpha,9-difluorobenzene-1,4-diene-3,20-diketone I crystal; (3) refining the 11 beta-hydroxyl-16 alpha,17-[(1-methyl ethylidene)-bis (oxygen)]-6 alpha,9-difluorobenzene-1,4-diene-3,20-diketone I crystal to obtain a fluocinolone acetonide finished product.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a method for preparing high-purity fluocinolone. Background technique [0002] Melasma, or melasma, is a common pigmented condition that primarily affects women during their reproductive years. Dark, mottled (hyperpigmented) macules can be seen on the face and neck, especially on the cheeks and forehead. Melasma is usually caused by hormonal activity from pregnancy or birth control pills. Hence, the condition is called "spots of pregnancy". The condition occurs when excess melanin deposits in the cells of the epidermis and dermis. Melasma can persist for a long time and often recurs during subsequent pregnancies. [0003] A compound topical preparation (containing hydroquinone, tretinoin and fluocinolone) was listed abroad in 2004 for the treatment of chloasma, and it has been recognized as the most effective drug for treating chloasma so far. In this compound preparation, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
CPCC07J71/0031
Inventor 张涛铸傅龙云王富军单含文王江君
Owner ZHEJIANG REACHALL PHARMA
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