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Preparation of prednisolone acetate

A technology of prednisolone acetate and prednisolone, which is applied in the direction of steroids and organic chemistry, can solve the problems of high toxicity of pyridine solvent, low product quality and high price, and shorten the production cycle and reaction time , the effect of improving the purity

Inactive Publication Date: 2015-07-08
HENAN LIHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The object of the present invention is to overcome the situation that adopts pyridine solvent to be big in the prior art, price is high and its product quality is not high, the yield of related technology is low, the quality is low, and a kind of preparation method of prednisolone acetate is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 1kg of prednisolone, 0.03kg of barium acetate, and 3L of dimethylformamide into a dry and clean reaction tank replaced with nitrogen three times in advance, stir to dissolve, and heat up to 30°C, then add 0.4 times of prednisolone Acetic anhydride with the weight of Songlong, heat preservation reaction for 3 hours, nitrogen protection throughout, keep anhydrous, TLC detection of complete reaction, pour into ice water pre-cooled to 0-10 ℃, stir for 30 minutes, filter and dry to obtain 1.10kg of acetic acid Prednisolone. The yield is 110.0%, the largest single impurity is 0.49%, and the total impurity is 0.92%.

Embodiment 2

[0015] Add 1kg of prednisolone, 0.06kg of barium acetate, and 4L of dimethylformamide into a dry and clean reaction tank replaced with nitrogen three times in advance, stir and dissolve, and heat up to 40°C, then add 0.6 times of prednisolone Acetic anhydride with the weight of Songlong, heat preservation reaction for 2.5 hours, protected by helium throughout the whole process, kept anhydrous, and TLC detected that the reaction was complete, poured into ice water that had been cooled to 0-10°C in advance, stirred for 30 minutes, filtered and dried to obtain 1.101 kg prednisolone acetate. The yield is 110.1%, the largest single impurity is 0.53%, and the total impurity is 0.98%.

Embodiment 3

[0017] Add 1kg of prednisolone, 0.1kg of barium acetate, and 4L of dimethylformamide into a dry and clean reaction tank replaced with nitrogen three times in advance, stir and dissolve, and heat up to 50°C, then add 1 times of prednisolone Acetic anhydride with the weight of Songlong, heat preservation reaction for 1 hour, nitrogen protection throughout the whole process, keep anhydrous, TLC detection of complete reaction, pour into ice water pre-cooled to 0-10 ℃, stir for 30 minutes, filter and dry to obtain 1.10kg prednisolone acetate. The yield is 110%, the largest single impurity is 0.52%, and the total impurity is 0.95%.

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Abstract

The invention discloses a preparation of prednisolone acetate and belongs to the technical field of chemical pharmacy. In the method, prednisolone and acetic anhydride are employed as raw materials for preparing the prednisolone acetate through a synthetic reaction which is carried out in a dipolar aprotic solvent. The prednisolone and the acetic anhydride are reacted with each other under an alkali metal acetate catalyst to prepare the prednisolone acetate, wherein the dipolar aprotic solvent is dimethyl formamide or dimethyl sulfoxide. According to the technical scheme, not only is a problem of toxicity due to pyridine solved, but also the yield and the quality are increased and the reaction time is reduced.

Description

technical field [0001] The invention relates to a preparation method of hormone drugs, in particular to a preparation method of prednisolone acetate, which belongs to the technical field of chemical pharmacy. Background technique [0002] Prednisolone acetate is an important adrenal glucocorticoid drug, mainly used for allergic and autoimmune inflammatory diseases, collagen diseases. Such as rheumatism, rheumatoid arthritis, lupus erythematosus, severe bronchial asthma, nephrotic syndrome, thrombocytopenic purpura, neutropenia, acute lymphoblastic leukemia, various adrenal insufficiency, exfoliative dermatitis, no blisters Sore neurodermatitis, eczema, etc. The main preparation technology of prednisolone acetate is made by the reaction of prednisolone and acetic anhydride, and traditional technology adopts pyridine as catalyst concurrently solvent to carry out reaction and prepares prednisolone acetate more, and there are following problems in this technology: [0003] 1. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
CPCC07J5/0053
Inventor 孟栋梁
Owner HENAN LIHUA PHARMA
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