Preparation method of fluocinonide

A technology of fluocinolone acetate and acid catalyst, applied in steroids, fermentation, organic chemistry, etc., can solve problems such as high environmental protection treatment costs of enterprises

Inactive Publication Date: 2018-01-23
TIANJIN JINYAO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of acid water will be produced in the dehydration process, whi

Method used

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  • Preparation method of fluocinonide
  • Preparation method of fluocinonide
  • Preparation method of fluocinonide

Examples

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Embodiment 1

[0095] Invention Example 1 Epoxy Reaction

Embodiment 1-1

[0097] Add 10g of chloride, 2ml of perchloric acid, and 120ml of acetone into the reaction flask, stir, cool down to 0°C, add 9g of NBS within 30 minutes, keep the reaction at 5-10°C, and monitor the reaction with thin-layer chromatography Process to the end of the reaction to obtain a halide, add 10% sodium carbonate aqueous solution to neutralize to pH = 6.5, raise the temperature to 20±2°C, add 15ml of 10% sodium hydroxide aqueous solution within 1 hour, and control the temperature at 20-25°C to react. Monitor the progress of the reaction by thin-layer chromatography until the end of the reaction, neutralize with acetic acid to pH=7, concentrate under reduced pressure until there is no acetone smell, dilute into ice water, filter, and dry to obtain 11.2 g of 9,11-epoxide.

Embodiment 1-2

[0099] Add 10g of chloride, 2ml of perchloric acid, and 50ml of tetrahydrofuran into the reaction flask, stir, cool down to 0°C, add 9g of NCS within 30 minutes, keep the reaction at 5-10°C, and monitor the reaction with thin-layer chromatography Process to the end of the reaction, dilute in water, filter to obtain the halide wet product, directly dissolve in 100ml of acetone, heat up to 20±2°C, add 15ml of 10% potassium hydroxide aqueous solution within 1 hour, and control the temperature at 20-25°C for reaction , monitor the progress of the reaction with thin-layer chromatography until the end of the reaction, neutralize the acetic acid to pH=7, concentrate under reduced pressure until there is no acetone smell, dilute into ice water, filter, and dry to obtain 10.9g of 9,11-epoxide.

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Abstract

The invention relates to a preparation method of fluocinonide, in particular to preparation of fluocinonide. The preparation method of the fluocinonide comprises the following steps: taking chloride as an initiator; and successively carrying out 9,11-epoxy, 1,2-dehydrogenation, 17-dehydration, 6-fluorination, 9,11-ring-opening, 16,17-position double-bond dihydroxy oxidation, 21-position esterification and 16,17-position condensation to obtain the fluocinonide. The novel process has high industrial value, side effects can be controlled effectively, and reaction yield and quality are improved; high-risk reaction is not involved in technological design, and industrialization is easy to implement; and high-pollution reaction does not exist, and environmental protection treatment pressure is relieved.

Description

technical field [0001] The invention relates to a new process for preparing fluocinolone acetate, which belongs to the technical field of pharmacy. Background technique [0002] Fluocinolone acetate, also known as fluocinolone acetate, chemical name 6α, 9α-difluoro-11β, 21-dihydroxy-16α, 17α-[(1-methylethylene) dioxy]pregna-1,4- Diene-3,20-diketone-21-acetate is a powerful topical anti-inflammatory glucocorticoid drug commonly used clinically, and is widely used in various dermatitis, eczema, psoriasis, lupus erythematosus, lichen planus and osteoarthritis Treatment of diseases such as arthritis. [0003] There are two main production process routes of fluocinonide acetate in the early days, respectively, fluocinonide acetate is prepared from epicortisol and mold oxide as starting materials. The two synthetic routes were put into production in the 1970s, and the process is relatively old. The oxides all use saponin as the starting material, and the supply of saponin is cur...

Claims

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Application Information

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IPC IPC(8): C07J71/00C07J13/00C07J7/00C12P33/20C12P33/02
Inventor 王淑丽张杰
Owner TIANJIN JINYAO GRP
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