US 12,264,145 B2
Crystal form F of trelagliptin and preparation method thereof
Kailin Xu, Guangzhou (CN); Jierui Huo, Guangzhou (CN); Jianping Wang, Guangzhou (CN); Shungquan Mu, Guangzhou (CN); and Suqing Zhao, Guangzhou (CN)
Assigned to GUANGDONG UNIVERSITY OF TECHNOLOGY, Guangzhou (CN)
Filed by GUANGDONG UNIVERSITY OF TECHNOLOGY, Guangzhou (CN)
Filed on Nov. 29, 2023, as Appl. No. 18/522,287.
Prior Publication US 2024/0199574 A1, Jun. 20, 2024
Int. Cl. C07D 401/04 (2006.01)
CPC C07D 401/04 (2013.01) [C07B 2200/13 (2013.01)] 2 Claims
 
1. A method for preparing a crystal form F of trelagliptin, comprising: adding a trelagliptin and a mediating protein to an agate ball-milling tank, adding agate mill balls, and conducting mechanical ball-milling at 10° C. to 40° C. for 0.5 h to 6 h to obtain the crystal form F of trelagliptin;
wherein an X-ray powder diffraction (XRPD) pattern of the crystal form F of trelagliptin has corresponding characteristic diffraction peaks at 2θ values of 11.47°, 12.41°, 13.21°, 14.46°, 16.13°, 16.93°, 17.40°, 18.49°, 19.24°, 19.80°, 20.37°, 21.76°, 22.76°, 23.21°, 23.75°, 25.08°, 25.52°, 26.02°, 28.02°, 29.54°, 30.92°, 34.12°, and 34.98°; and
a mass ratio of the trelagliptin to the mediating protein is (2-120):1.