Preparation method of propionic acid clobetasol

A technology of clobetasol propionate and a manufacturing method, which is applied in the manufacturing field of clobetasol propionate, can solve problems such as environmental pollution, unsafe production and operation, achieves high yield, low risk and hazard, The effect of simple reaction steps

Inactive Publication Date: 2007-03-07
ZHEJIANG DINGTAI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Method 2 Adding chromic acid during the reaction and recrystallizing with acetone-petroleum ether will pollute the environment, and organic solvents were not safe for production operations in the past
[0009] Since the environment and safe production have become an important issue now, the safety hazards in the production process or the pollution to the environment in the production process are prohibited. However, the effectiveness of this drug has not been replaced by another drug. , how to make the production process safe and pollution-free has become an urgent problem to be solved

Method used

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  • Preparation method of propionic acid clobetasol

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Embodiment 1

[0024] First, 13 kg of betamethasone 17-propionate sulfonate was mixed with 20 kg of anhydrous lithium chloride, dissolved in 100 kg of dimethylformamide (DMF), while the stirring speed was 100 rpm, and the mixing temperature was 95°C. The reaction time is 3 hours for chlorination reaction; second, after the chlorination reaction is complete, water analysis is carried out through 600 kg of ice water at a temperature of 10°C for 1 hour; 4000rpm, time 30 minutes, then at a temperature of 75 ° C, time 5 hours to dry after 11 kg of clobetasol propionate crude product; third, then dissolve the clobetasol propionate crude product in 150 kg of ethanol, and add 3 kg of activated carbon, decolorization, filtration, decolorization and filtration refers to heating temperature 50 ℃, time 1 hour, stirring speed 70rpm, stirring time 1 hour conditions, recovery of activated carbon; fourth, the filtrate is vacuum degree -0.08MPa, temperature 50 ℃, time 30 minutes, stirring speed 80rpm, stirri...

Embodiment 2

[0026] First, 13 kg of betamethasone 17-propionate sulfonate was mixed with 15 kg of anhydrous lithium chloride, dissolved in 100 kg of dimethylformamide (DMF), while the stirring speed was 100 rpm, and the mixing temperature was 90°C. The reaction time is 3 hours for chlorination reaction; second, after the chlorination reaction is complete, water analysis is carried out through 550 kg of ice water at a temperature of 8°C for 1 hour; 4000rpm, time 30 minutes, and then at a temperature of 80 ° C, after drying for 5 hours, 11 kg of clobetasol propionate crude product was obtained; thirdly, the clobetasol propionate crude product was dissolved in 140 kg of methanol, and added 3 kg of activated carbon, decolorization, filtration, decolorization and filtration refers to heating temperature 50 ℃, time 1 hour, stirring speed 70rpm, stirring time 1 hour conditions, recovery of activated carbon; fourth, the filtrate is vacuum degree -0.05MPa, temperature 50 ℃, time 30 minutes, stirrin...

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Abstract

The invention discloses a preparing method of chlorotestosterone betaprodine, which comprises the following steps: blending betamisong 17-propionic ester sulphonation and anhydrous lithium chloride with the rate at 1: 1-2; dissolving in the DMF to do chloridization reaction; elutriating through icy water; drying through centrifuging to obtain rough product; dissolving rough product in the carbinol or alcohol; adding activated charcoal; decoloring; filtering; recycling activated charcoal; condensing the filtrate; crystallizing; dehydrating; drying to obtain the product.

Description

technical field [0001] The invention relates to a medicine of clobetasol propionate, in particular to a preparation method of clobetasol propionate. Background technique [0002] Clobetasol propionate, chemical name: 16β-methyl-11β-hydroxy-17-(1-oxopropyl)-9-fluoro-21-chloro-pregna-1,4-diene-3 , 20-diketone [0003] The structural formula is: [0004] [0005] The molecular formula is: C 25 h 32 ClFO 5 ; Molecular weight: 466.97; Clobetasol propionate is currently the most powerful adrenal cortex hormone in the world. It is recorded in the Chinese Pharmacopoeia and other countries in the world because of its exact curative effect and safe use. It is widely used in external medicine and cosmetics and other fields, play a role in enhancing the curative effect. [0006] At present, there is no patent disclosure of the synthesis process of clobetasol propionate in China, and there is no literature report on the synthesis method. After consultin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00C07J75/00
Inventor 来明强徐建峰张利华钟斌强
Owner ZHEJIANG DINGTAI PHARMA
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