Mercaptopurine hemihydrate
View Patent ↗Provided herein is a new mercaptopurine form, as a hemihydrate, and methods of making and using the same.
1. Mercaptopurine hemihydrate.
2. The mercaptopurine hemihydrate of claim 1 having a dehydration temperature of greater than 200° C.
3. The mercaptopurine hemihydrate of claim 2 having a dehydration temperature of 240° C.
4. The mercaptopurine hemihydrate of claim 1 having at least 7 2Θ values selected from the group consisting of 10.59±0.1, 14.14±0.1, 15.86±0.1, 16.25±0.1, 18.83±0.1, 20.80±0.1, 20.42±0.1, 21.35±0.1, 24.93±0.1, 25.75±0.1, 26.02±0.1, 27.97±0.1, and 28.54±0.1°, as measured using CuKα radiation.
5. The mercaptopurine hemihydrate of claim 4 , having 2Θ values 10.59±0.1, 14.14±0.1, 15.86±0.1, 16.25±0.1, 18.83±0.1, 20.80±0.1, 20.42±0.1, 21.35±0.1, 24.93±0.1, 25.75±0.1, 26.02±0.1, 27.97±0.1, and 28.54±0.1°, as measured using CuKα radiation.
6. The mercaptopurine hemihydrate of claim 1 having a crystal structure as represented by the following parameters as measured at 85K: a (Å) 9.361, b (Å) 11.069, c (Å) 13.091, α(°) 90, β(°) 110.3, and γ(°) 90.
7. The mercaptopurine hemihydrate of claim 1 having a Raman spectrum with wavenumber shifts 444±2, 577±2, and 674±2 cm −1 , as measured using a 633 nm laser.
8. A method of making the mercaptopurine hemihydrate of claim 1 , comprising dissolving mercaptopurine monohydrate in methanol to form a methanol solution, contacting the methanol solution with water to form a solution, and crystallizing the mercaptopurine hemihydrate from the solution.
9. The method of claim 8 , wherein the ratio (parts per volume) of methanol to water in the solution is 100:1 to less than 2:1.
10. The method of claim 9 , wherein the ratio is 50:1 to 5:1.