Crystalline rostafuroxin
New crystalline forms of 17β-(3-Furyl)-5-βandrostane-3β,14β,17α-triol are described together with pharmaceutical composition containing the same and methods for their preparation. In particular new Forms B, C, D, E and H are here described.
1. A method for preparing crystalline, rostafuroxin Form F, consisting of dissolving rostafuroxin, amorphous, in ethanol to form a solution and then adding dropwise said solution to an excess of water at room temperature, and thereafter isolating crystalline rostafuroxin Form F having 2.5 moles of water per mole of rostafuroxin.
2. The method of claim 1 , wherein the amount of water used during crystallization is in excess of the amount of ethanol.
3. A method for preparing crystalline rostafuroxin Form F, consisting of:
dissolving amorphous or crystalline rostafuroxin, in ethanol to form a solution, adding said solution dropwise to an excess of water at room temperature to form a precipitate, filtering and isolating the precipitate, washing the isolated precipitate with water and drying it under vacuum to form crystalline rostafuroxin Form F having 2.5 moles of water per mole of rostafuroxin.
4. A method for preparing crystalline rostafuroxin Form F, consisting of
dissolving amorphous or crystalline rostafuroxin in ethanol to form a solution, adding said solution dropwise to an excess of water at room temperature, and thereafter isolating ciystalline rostafuroxin Form F having 2.5 moles of water per mole of rostafuroxin.
5. The method. of claim 1 , wherein the crystalline rostafuroxin Form F having 2.5 moles of water per mole of rostafuroxin has an X-ray diffraction spectrum as shown in FIG. 6 .
6. The method of claim 3 , wherein the crystalline rostafuroxin Form F having 2.5 moles of water per mole of rostafuroxin has an X-ray diffraction spectrum as shown in FIG. 6 .
7. The method of claim 4 , wherein the crystalline rostafuroxin Form F having 2.5 moles of water per mole of rostafuroxin has an X-ray diffraction. spectrum as shown in FIG. 6 .