Crystal of aldactone and preparation method thereof

Abstract

The invention discloses a crystal of aldactone and a crystallization preparation method thereof. X-ray powder has a characteristic peak at diffraction angles 2theta (which is equal to 8.2+ / -0.2, 9.8+ / -0.2, 10.0+ / -0.2, 12.8+ / -0.2, 13.6+ / -0.2, 13.8+ / -0.2, 15.4+ / -0.2, 16.0+ / -0.2, 16.5+ / -0.2, 16.8+ / -0.2, 18.1+ / -0.2, 18.8+ / -0.2, 21.3+ / -0.2, 22.0+ / -0.2, 24.0+ / -0.2 and 25.4+ / -0.2); at the temperature of 30-50 DEG C, aldactone solid is added into good solvent to obtain suspension of which the solution concentration is 0.3-1.0g / ml, and the suspension is put in an ultrasonic system to be processed by ultrasonic wave; poor solvent is added, temperature is lowered to 0-10 DEG C, and crystal grows for 1-5h; vacuum suction filtration, washing and drying are carried out to obtain an aldactone crystal product. A technology is simple, and a recovery rate is 90% or more.

Description

technical field [0001] The invention belongs to the technical field of medicine refining, in particular to a new crystal form of spironolactone and a preparation method thereof. Background technique [0002] The chemical name of Spironolactone is 17β-hydroxy-3-oxo-7α-(acetylthio)-17α-pregna-4-ene-21-carboxylic acid γ-lactone, and the CAS number is 52-01-7 , the molecular formula is C 24 h 32 o 4 S, relative molecular mass is 416.57, shown in its chemical structural formula (I). [0003] [0004] Spironolactone is a low potency diuretic with a structure similar to the natural adrenocortical hormone aldosterone. As a competitive inhibitor of aldosterone, spironolactone mainly acts on the collecting duct and distal convoluted tubule, blocking Na + -K + and Na + -H + exchange, resulting in Na + , Cl — and water excretion increased while K + , Mg 2+ and H + Excretion decreases, but for Ca 2+ and P 3— role is uncertain. Because spironolactone only acts on the di...

AI Technical Summary

Problems solved by technology

The solvents contained in the solvated compounds discovered so far are all organic solvents, which cannot be practically applied

At the same time, the stability of crystal form I is poor, so the crystal form II is mainly used in clinical treatment.

[0006] Most of the commercially available spironolactone products are mixed crystal forms of I crystal form and II crystal form (such as image 3 , 4 As shown), the ratio of the two crystal forms is difficult to control during the production process, the product stability is poor, and problems such as crystal form conversion may occur during storage; in addition, the currently existing products generally have small particle sizes (≤75μm), bulk density Small (0.30 / cm3), poor fluidity (angle of repose 49.5°), etc.

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