Method for preparing hydrocortisone acetate

A technology of hydrocortisone acetate and hydrocortisone, applied in organic chemistry, steroids, etc., can solve the problems of easy harm to the human body, flammable and explosive solvents, complex synthesis process, etc., and reach the key control point of the process Less, easy to operate, high yield effect

Active Publication Date: 2010-07-21
TIANJIN JINJIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its disadvantage is that pyridine is highly toxic, smells bad, and is easy to cause harm to the human body.
Although acetone, methyl ethyl ketone and other low-toxic solvents have been used instead ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put 160ml of DMSO into a three-neck flask, then add 20g of hydrocortisone, 10ml of acid anhydride, and then add 6ml of triethylamine, heat, stir and raise the temperature to 60°C, keep it warm for 4 hours, spot the plate to confirm that the reaction is complete, and pour the reaction solution into water , stirred, cooled to 10°C, and filtered after half an hour to obtain 20.4 g of hydrocortisone acetate. The yield is 102%, among which the largest single impurity is 0.82%, and the total impurity is 1.68%. Mp218°C.

Embodiment 2

[0020] Put 200ml of DMF into a three-neck flask, add 20g of hydrocortisone, 12ml of anhydride, and then add 30ml of piperidine, heat, stir and raise the temperature to 80°C, keep it warm for 2 hours, spot the plate to confirm that the reaction is complete, pour the reaction solution into water, and stir , cooled to 10°C, and filtered after half an hour to obtain 19.8g of hydrocortisone acetate. The yield is 99%, among which the largest single impurity is 0.85%, and the total impurity is 1.76%. Mp217°C.

Embodiment 3

[0022] Put 240ml of DMSO into a three-neck flask, put in 20g of hydrocortisone, 8ml of anhydride, and then add 20ml of ethylenediamine, heat, stir and raise the temperature to 50°C, keep it warm for 4 hours, spot the plate to confirm that the reaction is complete, pour the reaction solution into water, Stir, cool down to 10°C, and filter after half an hour to obtain 19.4 g of hydrocortisone acetate. The yield is 97%, among which the largest single impurity is 0.78%, and the total impurity is 1.62%. Mp218°C.

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PUM

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Abstract

The invention relates to a method for preparing hydrocortisone acetate. Three to twenty parts of dipolar aprotic solvent (including but not limited to dimethyl formamide or dimethyl sulfoxide and the like) is taken as the solvent, 0.1 to 1.5 parts of cheap organic amine (including but not limited to triethylamine, ethanediamine or piperidine and the like) is taken as the catalyst, one part of hydrocortisone and 0.4 to 1.0 part of acid anhydride react for 2 to 8 hours at 15 to 80 DEG C, and the hydrocortisone acetate can be prepared through adding water. The method replaces pyridine with low-toxic solvents, thereby reducing the environmental pollution and increasing the yield. The yield of the hydrocortisone acetate can reach more than 95 percent, the single maximum impurity is 0.82 percent, and the total impurity is 1.68 percent. The method stabilizes the product quality, reduces the cost, and is more suitable for large-scale industrialized production.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to a preparation method of hydrocortisone acetate. Background technique [0002] Hydrocortisone acetate is mainly used to treat rheumatoid arthritis, rheumatic fever, gout, and bronchial asthma. Injections are used for tuberculous or suppurative meningitis, tuberculous pleurisy, empyema, arthritis, tenosynovitis, tendon strain, sprains, prurigo nodosa, lichen planus, etc. Eye drops are used for various ophthalmic conditions. Creams are used for allergic or seborrheic dermatitis, pruritus, etc. Is an important corticosteroid drugs. [0003] Hydrocortisone acetate is mainly prepared by the reaction of hydrocortisone and acetic anhydride. Traditionally, pyridine is used as a solvent and catalyst for reaction to prepare hydrocortisone acetate. Its disadvantage is that pyridine is highly toxic, has an unpleasant smell, and is easy to cause harm to the human body. Co...

Claims

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Application Information

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IPC IPC(8): C07J5/00
Inventor 邵范武
Owner TIANJIN JINJIN PHARMA
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