Example 11
This experiment was designed to search further for a more stable form than Form I. Saturated and nearly saturated solutions of Compound 1 Di-Hydrochloric Acid Salt Form I were prepared at 50° C. and cooled in a bath slowly by using a programmed circulating bath. To the clear solution (8-10 mL) was added about 20-30 mg Compound 1 Di-Hydrochloric Acid Salt Form I to give a slurry. The formed slurry was then heated to 50° C. over 2 hours and then cooled down to 5° C. over 2 hours. This process was repeated for 3 days and the solid was filtered for further analysis. The results are presented in Table 15. Heating and cooling of the salt in methanol resulted in the new Form IX. PGP-72 TI
