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Preparation method of dexamethasone acetate

A technology of dexamethasone acetate and dexamethasone, applied in the direction of steroids, organic chemistry, etc., can solve the problem that the reaction solvent is difficult to handle, and achieve the effects of eliminating the need for temperature control procedures, high purity, and reduced pressure

Pending Publication Date: 2018-12-28
SHANDONG TAIHUA BIO & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method for the preparation method of dexamethasone acetate, which solves the problem that the reaction solvent is difficult to handle in the existing preparation process

Method used

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  • Preparation method of dexamethasone acetate

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Embodiment 1

[0018] A kind of preparation method of dexamethasone acetate that the present embodiment relates to, the reaction raw material dexamethasone of 10g is joined in the dimethyl sulfoxide reaction solvent of 30g, while stirring, add 10g sodium carbonate to adjust reaction solvent pH to be 7, Lower the temperature of the reaction solvent to 0°C, slowly add 10g of acetic anhydride dropwise, and react at a temperature of less than 15°C for 2-3 hours. TLC detects that there is no raw material point, and the reaction is completed. Add dexamethasone acetate into the water analysis tank. Control the temperature in the middle below 10 ℃, reduce the content of dexamethasone acetate in dimethyl sulfoxide, centrifuge finally and separate dexamethasone acetate, dry to get 10.5 grams of dexamethasone acetate crude product, crude product purity is 98.5%, receive The rate is 105%.

Embodiment 2

[0020] A kind of preparation method of dexamethasone acetate that the present embodiment relates to, the reaction raw material dexamethasone of 8g is joined in the dimethyl sulfoxide reaction solvent of 25g, while stirring, add sodium carbonate and adjust reaction solvent pH to be 8, will The temperature of the reaction solvent is lowered to 0°C, slowly add 8g of acetic anhydride dropwise, and react at a temperature of less than 15°C for 2-3 hours. TLC detects that there is no raw material point, and the reaction is completed. Add dexamethasone acetate into the water analysis tank. Control the temperature below 10°C to reduce the content of dexamethasone acetate in dimethyl sulfoxide, finally centrifuge to separate dexamethasone acetate, and dry to obtain 8.3 grams of dexamethasone acetate crude product, the crude product purity is 98.5%, and the yield 106%.

Embodiment 3

[0022] A kind of preparation method of dexamethasone acetate that this embodiment relates to, the reaction raw material dexamethasone of 12g is joined in the dimethyl sulfoxide reaction solvent of 35g, while stirring, add sodium carbonate to adjust reaction solvent pH to be 7.5, will The temperature of the reaction solvent is lowered to 0°C, slowly add 12g of acetic anhydride dropwise, and react at a temperature of less than 15°C for 2-3 hours. TLC detects that there is no raw material point, and the reaction is completed. Add dexamethasone acetate into the water analysis tank. Control the temperature below 10°C to reduce the content of dexamethasone acetate in dimethyl sulfoxide, finally centrifuge to separate dexamethasone acetate, and dry to obtain 12.7 grams of dexamethasone acetate crude product, the crude product purity is 98.5%, and the yield 106%.

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Abstract

The invention discloses a preparation method of dexamethasone acetate, and belongs to the technical field of pharmacy. The preparation method comprises the following steps: firstly adding 8-12 weightparts of a reaction raw material, namely hexadecadrol, to 25-35 weight parts of a dimethyl sulfoxide reaction solvent, and controlling the pH value of the reaction solvent to be 7-8; then dropwise adding 8-12 weight parts of acetic anhydride, performing a reaction under the condition that the temperature is lower than 15 DEG C, and when the hexadecadrol cannot be detected in a product, completingthe reaction; and finally, adding water, enabling the dexamethasone acetate to be separated out, reducing the temperature to 10 DEG C or below, lowering the content of the dexamethasone acetate in dimethyl sulfoxide, enabling the dexamethasone acetate to be isolated, and performing baking. Due to the adoption of the technology, environmental pollution is reduced, pressure for treating sewage by abiochemical method is reduced, besides, the cost of the reaction solvent is reduced, the product purity is high, the recovery rate is high, and the reaction temperature is automatically controlled.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a preparation method of dexamethasone acetate. It uses dimethyl sulfoxide and sodium carbonate, which are less harmful to biochemical bacteria, instead of pyridine as a reaction solvent, reducing the pressure and cost of raw materials for biochemical treatment of sewage. Background technique [0002] Dexamethasone and its series of products are long-acting adrenal cortex hormone drugs, which are widely used in clinical practice. Its products include: dexamethasone, dexamethasone acetate, dexamethasone sodium phosphate, etc. Among them, dexamethasone belongs to corticosteroid drugs, and dexamethasone and dexamethasone acetate are mainly used for collagen diseases, such as rheumatoid arthritis, lupus erythematosus, rheumatic heart disease, rheumatic fever, dermatomyositis, etc. Anti-inflammatory, anti-allergic, and anti-shock effects are more significant than predniso...

Claims

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Application Information

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IPC IPC(8): C07J5/00
CPCC07J5/0076
Inventor 王京沪
Owner SHANDONG TAIHUA BIO & TECH
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