Prednisolone dihydrate as well as preparation method and application thereof
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A technology of dihydrate and prednisolone, which is applied in the field of medicine, can solve problems such as high dehydration temperature, yellowing and deterioration of products, and high energy consumption, and achieve the effects of increasing yield, shortening time, and overcoming high temperature of baking material
Pending Publication Date: 2022-04-12
TIANJIN TIANYAO PHARM CO LTD +1
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Problems solved by technology
The dehydration temperature of sesquihydrate is high, the energy consumption is large, and it is easy to make the product yellow and deteriorate, so it is difficult to realize industrial production
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Embodiment 1
[0046] The preparation of embodiment 1 prednisolone dihydrate
Embodiment 1-1
[0048] Add 100g of crude prednisolone into a mixed solvent of methanol (200mL), dichloromethane (200mL) and purified water (60mL), heat to 35°C to dissolve and clarify, filter with suction to remove insoluble impurities, and use a constant pressure dropping funnel Add purified water (1000mL) to the mixture at a rate of 300mL / min for crystallization, mechanically stir for 1h, then cool down to 10°C at a rate of 30°C / h, filter with suction, and dry at 35°C to constant weight to obtain 97.2g of solid , the yield was 97.2%.
[0049] The obtained solid was analyzed by TG-DTA, and the weight loss was about 9.5%, which was confirmed to be prednisolone dihydrate. TG-DTA analysis such as figure 1 shown.
[0050] The obtained solid was subjected to X-ray diffraction measurement, and the measured characteristic peak positions were 2θ=7.2°±0.2°, 12.5°±0.2°, 14.2°±0.2°, 15.5°±0.2°, 16.2°±0.2°. X-ray diffraction measurements such as figure 2 shown.
[0051] The obtained solid was subj...
Embodiment 1-2
[0053] Add 100g of crude prednisolone into a mixed solvent of ethanol (1000mL), ethyl acetate (200mL) and purified water (200mL), heat to 75°C to dissolve and clarify, filter with suction, remove insoluble impurities, and use a constant pressure dropping funnel Add purified water (100mL) to the mixture at a rate of 200mL / min for crystallization, mechanically stir for 2h, then cool down to 0°C at a rate of 20°C / h, filter with suction, and dry at 33°C to constant weight to obtain 97.5g of solid , the yield was 97.5%.
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Abstract
The invention provides prednisolone dihydrate as well as a preparation method and application thereof, and relates to the technical field of medicines. The X-ray powder diffraction of the prednisolone dihydrate has characteristic peaks when the diffraction angle 2theta is equal to 7.2 degrees +/-0.2 degrees, 12.5 degrees +/-0.2 degrees, 14.2 degrees +/-0.2 degrees, 15.5 degrees +/-0.2 degrees and 16.2 degrees +/-0.2 degrees. The invention provides a brand-new prednisolone dihydrate, the dihydrate can be dehydrated and converted into a crystal form I at a lower temperature, compared with the existing method for preparing the crystal form I by using a sesquihydrate, the required time is greatly shortened to be within 5h from the original more than 24h, and the method overcomes the defects of high baking temperature, long period and yellowing and deterioration of a product, and has the advantages that the method is simple and convenient to operate, and the production cost is reduced. The requirements of industrial production can be met.
Description
technical field [0001] The invention relates to the technical field of medicine, in particular to a prednisolone dihydrate and a preparation method and application thereof. Background technique [0002] Prednisolone, English name: Prednisolone, is a commonly used adrenal cortex hormone, mainly used for allergic and autoimmune inflammatory diseases, collagen-derived diseases, such as rheumatism, rheumatoid arthritis, lupus erythematosus, Severe bronchial asthma, nephrotic syndrome, thrombocytopenic purpura, granulocytopenia, acute lymphoblastic leukemia, various adrenal insufficiency, exfoliative dermatitis, pemphigus, neurodermatitis, eczema, etc. Its structural formula is as follows: [0003] [0004] Prednisolone has three crystal forms, namely crystal form I, crystal form II and hydrate, wherein the hydrate is sesquihydrate (1.5H 2 O). The crystal forms of Form I and Form II are similar, but the crystal appearance of Form I is thinner than that of Form II in most ca...
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