FREE BASE CRYSTALLINE FORM OF A COMPLEMENT COMPONENT C5a RECEPTOR
a technology of complement components and free base crystalline forms, which is applied in the direction of antibody medical ingredients, drug compositions, immunological disorders, etc., can solve the problems of affecting the delivery efficiency of biologically relevant amounts of compound 1 and even potentially life-threatening consequences
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example 1
a Crystalline Form of Compound 1
[0068]Crude Compound 1 was prepared essentially as described in WO 2016 / 053890.
[0069]A crystalline form of Compound 1 was prepared by dissolving 18 g of crude Compound 1 in 50 mL acetone with heating at 40° C. (a concentration of about −0.36 g / mL). The warm solution was passed through a 10 μm polyethylene filter. The solution was then loaded into rotary evaporator at 30° C. bath temperature and 180 rpm rotational speed. The solid collected was dried further in a 45° C. oven for 1 hour. The XRPD data of the crystalline form is shown in FIG. 1, and the table of peaks measured are listed in Table 1, below.
TABLE 1Significant Peaks of Free Base Crystalline Form of Compound 1 Significant Peaks2-theta (deg)8.0620.288.4021.328.8822.3610.2022.6010.7223.1412.3523.4613.4424.4214.1024.6615.2125.0516.0525.4816.2026.2016.9226.4417.2827.1817.6427.6018.5828.7019.0029.2819.4429.60
example 2
ial Scanning Calorimetry (DSC) and Thermal Gravimetic Analysis (TGA) of the Free Base Crystalline Form of Compound 1
[0070]To evaluate the physical characteristics of the free base crystalline form of Compound 1, differential scanning calorimetry data was collected. Differential scanning calorimeter model DSC25 from TA Instruments˜ Waters LLC was used. Sample was weighed into a standard aluminum pan and sealed by a standard aluminum lid with pinhole. The measurement was completed by using 10° C. / min scanning rate, under a nitrogen purge. The DSC analysis determined that the free base crystalline form exhibits a melting (on set) of ˜213° C. and a endothermic peak at around 216° C. A plot of the DSC thermogram is shown in FIG. 2.
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