Ibrutinib solid forms and production process therefor
Provided are ibrutinib polymorphs, e.g., crystalline ibrutinib Forms III, IV, V, VI, VII, VIII and Form IX and processes for producing these crystalline forms, stable amorphous ibrutinib and processes for preparing stable amorphous ibrutinib, pharmaceutical compositions comprising these forms and methods of using these crystalline and amorphous forms.
1. A process for preparing amorphous ibrutinib, comprising:
dissolving ibrutinib in a solvent or mixture of solvents, optionally with heating;
loading the solution onto a chromatographic column,
eluting the ibrutinib from the column,
optionally concentrating the eluting solution,
spray drying the solution to give amorphous ibrutinib and
optionally drying the amorphous product.
2. The process of claim 1 , wherein said column is packed with silica.
3. The process of claim 1 , wherein the ibrutinib loaded into said column comprises ibrutinib form VII.
4. The process of claim 1 , wherein said eluting comprises a first step of eluting with a first solvent or mixture of solvents and a second step of eluting with a second solvent or mixture of solvents.