Crystal and deforming shaped smilagenin
A technology of smilagenin and smilagenin, which is applied in the directions of medical preparations containing active ingredients, steroids, organic chemistry, etc., can solve the problem that smilagenin is not described.
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Embodiment 1
[0140] Form I
[0141] A. Crystallization from acetone
[0142] Smilagenin (10.0 g) was suspended in acetone (250 ml) and the mixture was heated to reflux. The resulting solution was decanted, separated from some insoluble solids, and reheated to reflux to yield a clear solution. The solution was allowed to cool to 29°C for about 3.5 hours and further cooled gradually to 2°C with ice / water. The resulting solid was collected by filtration, washed with cold (5°C) acetone (50 ml) and dried in a vacuum oven for 3 days to obtain 7.4 g of pure smilagenin, which was characterized by XRPD as Form I according to our nomenclature .
[0143] B. Crystallization from Acetonitrile
[0144] A suspension of smilagenin (1.05 g) in acetonitrile (10 ml) was stirred overnight at ambient temperature. The solid was collected by filtration and dried in a vacuum oven at 80° C. to yield smilagenin Form I (0.92 g, 88% yield).
Embodiment 2
[0146] Form II
[0147] Smilagenin was produced by stereospecific reduction of diosgenin according to the method described in PCT Patent Application No. PCT / GB2003 / 001780 (WO-A-2004 / 037845).
[0148] XRPD was performed on smilagenin, and the pattern was found to be substantially similar to that shown in Figure 1 . On this basis, the material was characterized as Form II according to our nomenclature.
Embodiment 3 and 4
[0150] Form III
PUM
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