Process for the preparation of drospirenone as a fine powder through a double change of crystalline form
AssigneeIndustriale Chimica S.R.L.
InventorsRoberto Lenna, Michele Baldrighi
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Abstract
The present invention refers to a process for the industrial-scale preparation of 17β-hydroxy-6β,7β; 15β,16β-dimethylene-3-oxo-17α-pregn-4-ene-21-carboxylic acid γ-lactone, known by the common name of Drospirenone, in the form of a fine powder without the use of mechanical grinding or micronization techniques, but rather exploiting a double change of crystalline form, from Crystalline Form I to Crystalline Form II and from Crystalline Form II to Crystalline Form I. The invention also refers to the new Crystalline Form II of Drospirenone obtained in the process.
Claims11
A process for the production of 17β-hydroxy-6β,7β;15β,16β-dimethylene-3-oxo-17α-pregn-4-ene-21-carboxylic acid γ-lactone (Drospirenone) having fine particle size, characterized by a X90 value lower than 50 μm, through a double change of crystalline form:
- 1) From Crystalline Form I to Crystalline Form II, characterized by the presence in an XRPD spectrum of peaks at angles of 8.90°, 16.75° and 18.56°±0.2° 2θ;
- and
- 2) From Crystalline Form II to Crystalline Form I, characterized by the presence in an XRPD spectrum of peaks at angles of 12.30° and 17.35°±0.2° 2θ.
Drospirenone Crystalline Form II characterized by an X-ray diffractogram showing diffraction peaks at angular positions of 8.9°, 11.6°, 13.5°, 16.8°, 18.4°, 18.6°, 23.1°, 24.4° and 27.3°±0.2° 2θ.
Dependencies are inferred from the claim text.