Process for the preparation of crystalline form II of L-malic acid salt of sunitinib
The present invention relates to stable crystalline Form II of L-malic acid salt of sunitinib and its preparation.
1. A stable crystalline Form II of L-malic acid salt of sunitinib having an XRPD pattern wherein the characteristic d-spacing values are obtained substantially at 28.65, 14.40, 11.37, 9.59, 7.23, 6.09, 3.94, 3.70, and 3.30±0.3 degree 2θ.
2. The stable crystalline Form II of L-malic acid salt of sunitinib according to claim 1 , wherein the stable crystalline Form II of L-malic acid salt does not convert into any other solid form on storage of about 20 days or more.
3. The stable crystalline Form II of L-malic acid salt of sunitinib according to claim 1 , wherein the stable crystalline Form II of L-malic acid salt absorbs moisture to a level of not more than about 2%.
4. A process for the preparation of stable crystalline Form II of L-malic acid salt of sunitinib having an XRPD pattern wherein the characteristic d-spacing values are obtained substantially at 28.65, 14.40, 11.37, 9.59, 7.23, 6.09, 3.94, 3.70, and 3.30±0.3 degree 2θ, wherein the process comprises:
a) charging a solution of L-malic acid salt of sunitinib in a solvent to a spray dryer;
b) removing the solvent from the solution obtained in step a) by spray drying; and
c) collecting stable crystalline Form II of L-malic acid salt of sunitinib from the spray dryer.
5. The process according to claim 4 , wherein the solvent is water, an alkanol, or a mixture thereof.
6. The process according to claim 5 , wherein the alkanol is methanol.
7. The stable crystalline Form II of L-malic acid salt of sunitinib of claim 3 , wherein the crystalline form is produced by spray drying.
8. The stable crystalline Form II of L-malic acid salt of sunitinib of claim 7 , wherein the spray drying comprises spray drying a solution of L-malic acid salt of sunitinib in a solvent.
9. The stable crystalline Form II of L-malic acid salt of sunitinib of claim 8 , wherein the solvent comprises water, an alkanol, or a mixture thereof.
10. The stable crystalline Form II of L-malic acid salt of sunitinib of claim 9 , wherein the alkanol comprises methanol.
11. A spray dried stable crystalline Form II of L-malic acid salt of sunitinib according to claim 3 .