Isopropanol → SHR-1258 dimaleate

Participants

Reaction Steps

1.0 g of SHR1258 (prepared according to PCT Patent Application Publication WO2011029265) and 0.4 g of maleic acid were dissolved in 25 ml of isopropyl alcohol by heating. A solid was present while refluxing. After removing from heating, the obtained mixture was stirred to cause a precipitate. The resulting precipitate was collected by filtration and then dried at 45° C. under vacuum overnight to obtain 0.85 g of SHR1258 dimaleate crystal. Yield: 60%. X-ray diffraction pattern is shown in FIG. 1 in which there are characteristic peaks at 6.28 (14.06), 6.74 (13.10), 10.60 (8.34), 11.58 (7.64), 13.50 (6.55), 14.90 (5.94), 15.80 (5.60), 18.26 (4.85), 20.66 (4.30), 21.14 (4.20), 22.96 (3.87), 24.34 (3.65), 25.54 (3.49), and 26.12 (3.41). The DSC pattern is shown in FIG. 2, with a sharp heat absorption peak at 131.429° C. The crystal was defined as form I crystal.

Provenance & Evidence