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Preparation method of prednisolone hydrate

A single technology of prednisolone and prednisolone, applied in a new preparation field, can solve the problems of research, long crystallization time, single method, etc., and achieve the effect of shortening time and improving yield

Active Publication Date: 2011-06-01
TIANJIN JINYAO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Regarding the preparation of prednisolone hydrate, the method of using methanol water to prepare prednisolone hydrate in the document GB836747A is single, and the crystallization time is long and the yield is low etc. Insufficient; 16 hours when preparing prednisolone hydrate in embodiment one, yield is 84.9%; And yield is only about 30% in embodiment 2
The main reason for this is that the literature GB836747A has little research on the influencing factors of solvent selection, water addition, temperature, etc., and there is no systematic preparation method research.

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  • Preparation method of prednisolone hydrate
  • Preparation method of prednisolone hydrate
  • Preparation method of prednisolone hydrate

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Effect test

Embodiment 1

[0025] After 1g of prednisolone was completely dissolved in 10mL of ethanol at 75°C, 20mL of water was added, and then the temperature was lowered to room temperature (25°C) at a rate of 0.1°C / min; 0.92g of prednisolone hydrate crystals were precipitated. The resulting product was dried in an infrared oven under normal pressure for 12 hours, and tested by the Karl Fischer method, the moisture content was 6.53%.

[0026] The obtained crystals were subjected to X-ray powder diffraction measurement, and the measured characteristic peak positions were d=6.20, 5.76, 5.09, 4.39, 3.94, 3.71, 3.47, 3.36, 3.02.

Embodiment 2

[0028] Dissolve 1g of prednisolone with 10mL of THF at 45°C, add 15mL of water, and then evaporate at 60°C for 3h; 0.89g of prednisolone hydrate crystals are precipitated. The resulting product was dried in an infrared oven under normal pressure for 12 hours, and tested by the Karl Fischer method, the moisture content was 6.15%.

Embodiment 3

[0030] Add 1g of prednisolone into 6mL of dioxane, heat to reflux, dissolve, slowly add 10mL of water, and then cool down to room temperature (25°C) at a rate of 0.1°C / min; the precipitated prednisolone is hydrated 0.90 g of crystallized material. Tested by Karl Fischer method, the moisture content is 6.35%.

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Abstract

The invention relates to a preparation method of prednisolone hydrate. The preparation method is as follows: a) forming mixed organic aqueous solution of water and organic solvents of the prednisolone hydrate, wherein the organic solvents are selected from one or more of acetonitrile, dioxane, ethanol and tetrahydrofuran (THF); and b) carrying out precipitation crystallization on the solution in the step a through conventional crystallization methods, wherein the conventional crystallization methods comprise a cooling method and a solvent evaporation method.

Description

Field of invention: [0001] The present invention relates to a kind of crystallization technology of steroid drug, especially a kind of new preparation method of prednisolone hydrate. Background technique: [0002] The chemical structure of Prednisolone sesquihydrate (CAS: 52438-85-4) is as follows: [0003] [0004] Prednisolone is a commonly used adrenocortical hormone, mainly used for allergic and autoimmune inflammatory diseases, collagen-derived diseases, such as rheumatism, rheumatoid arthritis, lupus erythematosus, severe bronchial asthma, nephrotic syndrome Syndrome, thrombocytopenic purpura, granulocytopenia, acute lymphoblastic leukemia, various adrenal insufficiency, exfoliative dermatitis, pemphigus, neurodermatitis, eczema, etc. [0005] Prednisolone hydrate has been recorded in the United States Pharmacopoeia at present, see USP31 edition United States Pharmacopoeia page 3061, wherein the requirement for hydrate is that the percentage of weight loss on dryin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
Inventor 何运良李金禄
Owner TIANJIN JINYAO GRP