Iguratimod crystal form and its composition
A technology of crystal form and composition, which is applied in the field of autoimmune regulation drugs to achieve the effect of high biological activity and easy production
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[0081] Example 1. Preparation of Form 1: Take 10 g of Iramod into a 2000 ml round-bottomed flask, add 1000-1500 ml analytically pure ethanol and activated carbon, heat, reflux, and filter. The filtrate is placed at room temperature for 18 hours, filtered, and filtered. The cake was washed and dried under reduced pressure at 50-60°C to obtain 9.8 g of Form 1, with a melting point of 237-238°C.
[0082] The XRD pattern of form 1 has peaks at about 26.00, about 24.56, about 20.80, about 19.56, about 17.54, about 10.92 and about 6.88, and its DSC endothermic transition is about 236-240°C; the infrared absorption spectrum (IR) (KBr, cm -1 ) At approximately 3342, 3276, 3123, 3065, 2869, 1687, 1621, 1531, 1489, 1425, 1358, 1264 and 1156cm -1 There are characteristic bands, see Figure 1-3.
Example Embodiment
[0083] Example 2. Preparation of Form 2: Take 10 grams of Iramud into a 1000 ml round-bottomed flask, add 500-1000 ml analytically pure acetonitrile and activated carbon, heat, reflux, and filter. The filtrate is placed at room temperature for 24 hours, filtered, and filtered. The cake was washed and dried under reduced pressure at 50-60°C to obtain 9.5 g of Form 2. Melting point: 237-238°C.
[0084] The XRD pattern of form 2 is about 24.48, about 22.60, about 21.76, about 19.52, about 10.84, about 18.08, about 17.56, about 16.92, about 11.20, about 9.36, about 8.64, about 7.48, about 6.84, about 6.52, and about 5.60. Peak, the DSC endothermic transition is about 236-240℃; the IR (KBr, cm -1 ) At approximately 3342, 3276, 3123, 3065, 2869, 1687, 1621, 1531, 1489, 1425, 1358, 1264 and 1156cm -1 There are characteristic bands, differential thermal analysis chart, and infrared spectrum are the same as form 1, see Figure 2-3.
Example Embodiment
[0085] Example 3. Preparation of Form 3: Take 10 g of Iramod into a 100 ml round-bottomed flask, add 20 ml analytically pure dimethylformamide and activated carbon, heat, reflux, and filter. The filtrate is placed in a refrigerator at room temperature for 18 hours. Filter, wash the filter cake, and dry under reduced pressure at 50-60°C to obtain 9.5 g of Form 3. Melting point: 237-238°C.
[0086] The XRD pattern of Form 3 has peaks at approximately 27.28, approximately 25.68, approximately 25.24, approximately 24.40, approximately 24.04, approximately 23.08, approximately 20.16, approximately 17.52, approximately 10.56, and approximately 6.00, and its DSC endothermic transition is approximately 236-240°C; IR(KBr, cm -1 ) At approximately 3342, 3276, 3123, 3065, 2869, 1687, 1621, 1531, 1489, 1425, 1358, 1264 and 1156cm -1 There are characteristic bands, differential thermal analysis chart, and infrared spectrum are the same as form 1, see Figure 2-3.
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