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Preparation method of prednisolone acetate

A technology of prednisolone acetate and acidic conditions is applied in the field of preparation of steroid compounds, which can solve the problems of complicated operation, easy decomposition, unstable intermediates and the like, and achieves simple separation and purification operation, high material utilization rate, The effect of low cost of raw materials

Inactive Publication Date: 2013-11-20
WUHAN LANGJI TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, chromium is used in the reduction step, which causes heavy metal residues; in addition, the cost of iodo is relatively high, and the intermediate is unstable and easy to decompose, so it must be stored in the dark under nitrogen; during this period, the intermediate is separated many times, and the operation is complicated. Facilitate large-scale industrial production

Method used

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  • Preparation method of prednisolone acetate
  • Preparation method of prednisolone acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Add 10g of raw material (I), 50ml of acetone, and 20ml of glacial acetic acid into the reactor, stir, cool down to 0°C, add 30ml of acetone dissolved with 9g of NBS within 30 minutes, and react at 5-10°C for 2 hours. Acetone was distilled off.

[0034] (2) Add 30-50ml of ether into the reactor, slowly add 3.8g-4.2g of zinc powder, and carry out the reduction at room temperature for 2h. Stirring was continued for 15 minutes after the end of the TLC detection reaction.

[0035] (3) Add 0.1g catalyst AlCl to the reactor 3 , Stir at -5~0°C, slowly add 30ml of diethyl ether solution containing 5.5g of bromine within 30 minutes; keep the reaction temperature constant, and react for 2h.

[0036] (4) Ether is evaporated and recovered, and the acetone evaporated in step (1) is added as a solvent; 24g of sodium hydroxide powder is added to the reactor, and then 3ml of triethylamine is added, heated to 50-55°C under stirring for reaction 3 Hours, TLC detects the end of the ...

Embodiment 2

[0039] Also using 10 g of the compound of formula I as a raw material, the method in Example 1 was used to carry out steps (1) to (3);

[0040] (1) Add raw material (I) 10g and 50ml acetone, 20ml glacial acetic acid to acid-resistant reactor 1, stir, cool down to 0°C, add 30ml of acetone dissolved with 9g NBS within 30 minutes, and react at 5-10°C 2 hours. Acetone was distilled off.

[0041] (2) Add 30-50ml ether to reactor 1, slowly add zinc powder, and carry out reduction at room temperature for 2 hours. Stirring was continued for 15 minutes after the TLC reaction was completed.

[0042] (3) Add 0.2g catalyst AlCl to reactor 1 3 , Stir at -5~0°C, slowly add 30ml of diethyl ether solution containing 5.5g of bromine within 30 minutes; keep the reaction temperature constant, and react for 2h.

[0043] (4) Add sodium hydroxide to the reactor 1 to adjust the pH to neutral, then the zinc salt will precipitate out, filter the solution to remove the insoluble matter, wash the pr...

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PUM

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Abstract

The invention relates to a synthesis method of prednisolone acetate. A compound disclosed as Formula I is subjected to double bond bromination, reduction debromination, bromization and replacement reaction to generate prednisolone acetate. The method provided by the invention is high in yield, simple to operate and suitable for industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of steroid compound, especially relate to the preparation of prednisolone acetate. Background technique [0002] Prednisolone acetate is the acetate of prednisolone, English name Prednisolone Acetate, chemical name: 11β, 17α, 21-trihydroxypregna-1,4-diene-3,20-dione-21- Acetate, molecular structure see formula V in the reaction formula. [0003] Prednisolone acetate is white or off-white crystalline powder; odorless, bitter, slightly soluble in methanol, ethanol or chloroform, almost insoluble in water. [0004] Prednisolone acetate is a glucocorticoid drug used externally to treat allergic, non-infectious skin diseases and some proliferative skin diseases. Such as dermatitis, eczema, neurodermatitis, seborrheic dermatitis and pruritus. For allergic and autoimmune inflammatory diseases, collagen diseases. Such as rheumatism, rheumatoid arthritis, lupus erythematosus, severe bronchial ast...

Claims

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Application Information

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IPC IPC(8): C07J5/00
Inventor 李竞
Owner WUHAN LANGJI TECH DEV
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