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Preparation method of triketone dehydrogenation product

A triketone and dehydrogenation technology, applied in the field of preparation of triketone dehydrogenates, can solve the problems of large environmental pollution and low efficiency, and achieve the advantages of reducing side reactions, improving operating conditions, excellent stereoselectivity and regioselectivity. Effect

Pending Publication Date: 2022-03-18
HENAN LIHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, 17α-hydroxypregn-4-ene-3,11,20-trione dehydrogenation is an important part in the synthesis of deflazacort. The traditional dehydrogenation method is chemical dehydrogenation, which has low efficiency and is environmentally friendly. big pollution problem

Method used

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  • Preparation method of triketone dehydrogenation product
  • Preparation method of triketone dehydrogenation product
  • Preparation method of triketone dehydrogenation product

Examples

Experimental program
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Effect test

Embodiment 1

[0051] S11, mixing the triketone and water with a mass ratio of 1:2, then stirring and beating at a stirring speed of 100r / min, the stirring and beating time is 60min, to obtain a slurry;

[0052] Add polyether defoamer dispersant to the slurry, and the mass ratio of slurry to dispersant is 1:0.01. After stirring and mixing, heat up to 121°C to sterilize for 25 minutes, then cool down to room temperature to obtain triketone slurry;

[0053] S12, first add 4% methanol to the fermentation culture liquid, and after 1 hour, put the processed slurry into the fermentation culture liquid of Arthrobacter simplex twice, and the total concentration of the slurry is 3% of the fermentation culture liquid, wherein , the first feeding amount accounted for 20% of the total feeding amount, after 24 hours, the remaining slurry was added, and cultured at 30°C and 150 r / min for 48 hours to obtain triketone dehydrogenation.

Embodiment 2

[0055] S21, mixing the triketone and water at a mass ratio of 1:3, then stirring and beating at a stirring speed of 150r / min, the stirring and beating time is 20min, to obtain a slurry;

[0056] Add Tween 80 dispersant to the slurry, and the mass ratio of slurry to dispersant is 1:0.05. After stirring and mixing, heat up to about 121°C for sterilization for 25 minutes, and then cool down to room temperature to obtain a triketone slurry;

[0057] S22, first add 5% ethanol to the fermentation culture liquid, after 1h, put the processed slurry into the fermentation culture liquid of Arthrobacter simplex in 2 times, the total concentration of the slurry is 3% of the fermentation culture liquid, wherein , the first feeding amount accounted for 40% of the total feeding amount, after 30h, the remaining slurry was added, and cultivated for 32h under the conditions of 32°C and 150r / min to obtain triketone dehydrogenation.

Embodiment 3

[0059] S31, mixing the triketone and water with a mass ratio of 1:2, then stirring and beating at a stirring speed of 130r / min, the stirring and beating time is 30min, to obtain a slurry;

[0060] Add Tween 80 dispersant to the slurry, and the mass ratio of slurry to dispersant is 1:0.03. After stirring and mixing, heat up to about 121°C for sterilization for 25 minutes, and then cool down to room temperature to obtain a triketone slurry;

[0061] S32, first add 4% methanol to the fermentation culture liquid, and after 2 hours, put the processed slurry into the fermentation culture liquid of Arthrobacter simplex twice, and the total concentration of the slurry is 4% of the fermentation culture liquid, wherein , the first feeding amount accounted for 30% of the total feeding amount, after 25h, the remaining slurry was added, and cultivated for 40h under the conditions of 34°C and 150r / min to obtain triketone dehydrogenate.

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Abstract

The invention relates to the technical field of pharmacy, in particular to a preparation method of a triketone dehydrogenation product, which comprises the following steps: mixing, stirring and pulping a triketone product and water to obtain slurry; adding a dispersing agent into the slurry, and sterilizing at high temperature to prepare triketone slurry; wherein the mass ratio of the triketone substance to the water is 1: (2-3); the mass ratio of the slurry to the dispersing agent is 1: (0.01-0.05); putting the triketone slurry into a fermentation culture solution of arthrobacter simplex for biotransformation in batches to obtain a triketone dehydrogenation product; wherein the total adding concentration of the triketone slurry is 2-4% of that of the fermentation culture solution. The biotransformation method can specifically remove 1, 2 hydrogen of 17 alpha-hydroxypregna-4-ene-3, 11, 20-triketone and introduce double bonds, the transformation rate is as high as 90%, the use of strong acid, strong alkali and toxic and harmful chemicals is avoided or reduced, the operation conditions are improved, the production cost is reduced, and the concept of green development is met.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a preparation method of a triketone dehydrogenate. Background technique [0002] Deflazacort is a steroidal anti-inflammatory drug, which is a white or off-white crystalline powder, which belongs to adrenocorticotropic hormone and adrenocorticotropic hormone drugs. It has pharmacological effects such as anti-inflammatory, anti-endotoxin, and immune suppression. 10-20 times of Songlong, 40 times of hydrocortisone. It has a very important role in clinical practice, and can be used for emergency treatment of critical illnesses, and is suitable for hypofunction of the adrenal cortex, autoimmune diseases, etc. [0003] Among them, the 1,2-position dehydrogenation process is a key step in the production process of deflazacort, which has an important impact on the quality and yield of deflazacort. However, 17α-hydroxypregn-4-ene-3,11,20-trione dehydrogenation is an important part in ...

Claims

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Application Information

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IPC IPC(8): C12P33/02C12N1/20C12R1/06
CPCC12P33/02C12N1/20
Inventor 张海涛牛国栋王国永
Owner HENAN LIHUA PHARMA
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