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A kind of high-yield spironolactone fine preparation method
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A spironolactone and high-yield technology, which is applied in the field of high-yield spironolactone high-quality preparation, can solve the problems of low refining yield and spironolactone yield, and achieve the effect of improving the refining yield and reducing the content of impurities
Active Publication Date: 2021-11-30
ZHEJIANG SHENZHOU PHARMA
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[0007] In order to solve the problem of low yield of spironolactone, we found that the main reason is that spironolactone will be degraded into canrenone during the refining process, resulting in low refining yield
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Embodiment 1
[0026] Put 10g of canrenone into 10ml of thioacetic acid, add 100ml of methanol, reflux for 3 hours, cool down to 0°C, filter to get the crude spironolactone, put the crude spironolactone into 50ml of ethanol, add 0.01g of pyridine, and then add 0.2g of activated carbon , after the decolorization finishes, filter out gac, concentrate, filter, dry to obtain 9.9g spironolactone fine work, yield 99%, HPLC sees attached figure 1 , from attached figure 1 It can be seen that the purity of the obtained spironolactone refined product is 98.593%, and the impurity canrenone content is 0.232%.
Embodiment 2
[0028] Put 10g of canrenone into 5ml of thioacetic acid, add 50ml of methanol, reflux for 2 hours, cool down to 0°C, filter to get the crude spironolactone, put the crude spironolactone into 300ml of methanol, add 0.05g of triethylamine, and then add 0.5 g activated carbon, after the decolorization finishes, filter the activated carbon, concentrate, filter, and dry to obtain 9.9g spironolactone fine product, the yield is 99%, and the purity is 99.5%.
Embodiment 3
[0030] Put 10g of canrenone into 8ml of thioacetic acid, add 80ml of methanol, reflux for 5 hours, cool down to 0°C, filter to obtain the crude spironolactone, put the crude spironolactone into 15ml of dichloromethane and 15ml of acetone, add 0.1g1,8 -diazabicycloundec-7-ene (DBU), then add 1g of gac, filter gac after decolorization, concentrate, filter, dry to obtain 9.8g spironolactone fine product, yield 98%, purity 99.4%.
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Abstract
The invention discloses a preparation method of a high-yield spironolactone refined product, which belongs to the technical field of medicine preparation and processing. The method uses canrenone as a raw material, reacts with methanol and thioacetic acid to obtain a crude spironolactone, dissolves the crude spironolactone in a solvent, adds a stabilizer, then adds activated carbon, decolorizes, filters out the activated carbon, concentrates and refines to obtain a fine spironolactone. The method of the invention adds a stabilizer in the decolorization process to prevent the spironolactone from degrading into impurities during the decolorization process, improves the yield, has extremely high commercial competitiveness, is suitable for large-scale industrial production, and has good economic benefits.
Description
technical field [0001] The invention relates to the technical field of preparation and processing of medicines, in particular to a preparation method of high-yield spironolactone refined products. Background technique [0002] Spironolactone is a weak potassium-sparing diuretic, also known as spironolactone and spironolactone. It is a white or off-white fine crystalline powder with a slight bitter taste, odorless or a slight thiolodor. Easily soluble in chloroform, insoluble in water, soluble in ethanol, soluble in benzene or ethyl acetate. The chemical structure is similar to that of aldosterone, which can compete with aldosterone for the aldosteronereceptor in the cytoplasm of the distal convoluted tubule and collecting duct, affecting the binding of aldosterone to the receptor, thus hindering the synthesis of aldosterone-induced protein, thereby inhibiting the K+-Na+ exchange and reducing the excretion of potassium , play a potassium-sparing diuretic effect. [0003] ...
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