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The preparation method of deflazacort

A technology of defluket and organic solvent, which is applied in the field of preparation of steroid hormone drugs, can solve the problems of the increase of production cost and market price of deflukete, the increase of production cost of saponin and mold removal, the increase of planting cost, and the like. High product yield, favorable for industrial production and short synthesis route

Active Publication Date: 2018-02-23
HUNAN KEREY BIOTECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Its synthetic route is long, and the total yield of synthesis is low, and the extraction of diosgenin and subsequent multi-step synthetic chemical reactions produce more waste water, which is not easy to handle and easily pollutes the environment
More importantly, with the depletion of wild yam plant resources, and the artificial planting of yam plants, due to the increasing cost of labor and fertilizers, the production costs of saponin and mildew have increased exponentially, resulting in defucort The substantial increase in production costs and market prices has had a significant impact on the global market for deflazacort

Method used

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  • The preparation method of deflazacort
  • The preparation method of deflazacort

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A: Preparation of hydroxylamine

[0020] In a 1000ml three-necked bottle, add 20g 16(17)a-epoxyprednisolone, 30ml DMF, 300ml chloroform, keep warm at 30-35℃, stir and pass in 8g ammonia gas, and react under 1-2 atmospheric pressure After 16 to 20 hours, TLC detects the end point of the reaction. After the reaction, exhaust the ammonia gas in a vacuum, add 3x100ml saturated saline to wash 3 times, then add 100ml pure water to wash once, then concentrate chloroform under reduced pressure to dryness, and add 200ml acetic acid Ethyl ester, 1g activated carbon, stirred and refluxed for 60-90 minutes, cooled to 50-55 degrees, suction filtered while hot, washed carbon with 1-2ml ethyl acetate, combined filtrate and washing liquid, and then concentrated under reduced pressure below 50°C to obtain 95 % ethyl acetate, cool the system to -5-0°C, stir and crystallize for 2 to 3 hours, filter with suction, wash with 0.5-1ml ethyl acetate, combine the lotion and filtrate and set up a...

Embodiment 2

[0024] A: Preparation of hydroxylamine

[0025] In a 1000ml three-necked bottle, add 20g 16(17)a-epoxyprednisolone and 120ml toluene, keep warm at 30-35°C, stir and pass in 8g of ammonia gas, and react at 1-2 atmospheric pressure for 16-20 hours , TLC to detect the end point of the reaction. After the reaction, exhaust the ammonia in a vacuum, add 3x50ml saturated saline to wash, then add 50ml of pure water to wash, then, concentrate toluene under reduced pressure to dryness, add 200ml of ethyl acetate, 1g of activated carbon, and stir to reflux After 60-90 minutes, cool down to 50-55°C, suction filter while it is hot, wash the carbon with 1-2ml ethyl acetate, combine the filtrate and washing liquid, and then concentrate under reduced pressure below 50°C to obtain 95% ethyl acetate. Cool to -5-0°C, stir and crystallize for 2 to 3 hours, filter with suction, wash with 0.5-1ml ethyl acetate, combine the lotion and filtrate and set up a batch; dry the filter cake below 70°C to ob...

Embodiment 3

[0029] A: Preparation of hydroxylamine

[0030]In a 1000ml three-necked bottle, add 20g 16(17)a-epoxyprednisolone and 120ml ethanol, keep warm at 30-35°C, stir and feed 8g of ammonia gas, and react at 1-2 atmospheric pressure for 16-20 hours, TLC detects the end point of the reaction. After the reaction, the ammonia gas is exhausted in vacuum, the ethanol is concentrated under reduced pressure to nearly dryness, the temperature is lowered, 300ml of chloroform is added, the residue is stirred to dissolve, and then 3x100ml of saturated saline is added for washing, followed by 100ml of pure water for washing. , Concentrate chloroform to dryness under reduced pressure, add 200ml ethyl acetate, 1g activated carbon, stir and reflux for 60-90 minutes, cool to 50-55°C, suction filter while hot, wash carbon with 1-2ml ethyl acetate, combine filtrate and lotion , then concentrate under reduced pressure below 50°C to get 95% ethyl acetate, cool the system to -5-0°C, stir and crystallize ...

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Abstract

Provided is a method for preparing deflazacort. The method comprises the steps that 16(17)-epoxy prednisolone synthesized through 4AD is adopted as a raw material, and hydroxylamine matter is firstly synthesized, wherein 16(17)a-epoxy prednisolone and dammonia gas react for 16-18 hours in an organic solvent at the temperature of 10 DEG C to 50 DEG C and 1-2 barometric pressures, and treatment is carried out to obtain the hydroxylamine matter 17a-amidogen and 16a- hydroxyl-prednisolone; the hydroxylamine matter and acetic anhydride are catalyzed with acid in an organic solvent to react for 6-8 hours at the temperature of 10 DEG C to 50 DEG C, and treatment is carried out to obtain crude deflazacort; ethyl alcohol and activated carbon are used for decoloration and refining to obtain the deflazacort product. The HPLC content is 99.0% or above, the melting point ranges from 255 DEG C to 256 DEG C, and the synthesis weight total recovery ranges from 80% to 85%. The raw material is cheap and available, process operation is easy and convenient, the synthesis route is short, the product yield is high, and the production cost can be remarkably reduced; the reaction solvent is recycled and used cyclically and indiscriminately, and the method is economical, environmentally friendly and very suitable for industrial production.

Description

technical field [0001] The invention belongs to the preparation technology of steroid hormone medicine, and specifically refers to a preparation method for synthesizing deflazacort by two-step reaction. Background technique [0002] Deflazacort (molecular formula C23H29NO4) is a third-generation steroidal glucocorticoid drug, which is mainly used clinically for primary and secondary adrenal cortical insufficiency, rheumatism, collagen disease, skin disease, fulminant and The treatment of disseminated tuberculosis, hematopoietic system diseases, ulcerative colitis, hematopoietic system nausea and many other diseases has low side effects, good effect and broad market prospect. The traditional production method of Defucort is to use diosgenin extracted from yam plant, through six steps of chemical reaction, and two steps of microbial fermentation to obtain an important hormone drug intermediate—mold dehydrogenation product (referred to as mold dehydrogenation) as raw material. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
CPCC07J71/0068
Inventor 胡爱国谢来宾吴来喜
Owner HUNAN KEREY BIOTECH
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