Crystal form of lornoxicam and preparation method thereof
A technology of lornoxicam and crystal form, applied in organic chemistry methods, organic chemistry and other directions, can solve problems such as poor stability of lornoxicam crystal form
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Embodiment 1
[0037] Add 4.00g of lornoxicam solid and 63.16g of acetone into the four-necked reaction flask, start stirring, start heating after stirring and mixing, and add 5wt.% potassium hydroxide aqueous solution and 5wt.% triethylamine aqueous solution under the temperature control at 20°C The pH value was adjusted to 8, the reaction system was dissolved, and stirring was continued at 30° C. for 30 minutes after dissolution. Slowly add 10wt.% acetic acid aqueous solution to the clarified solution to adjust the pH figure 2 The crystal morphology under the electron microscope is shown in Figure 5 shown. Table 1 shows the typical characteristic absorption peaks at the diffraction angle 2θ of the X-ray powder diffraction pattern of this crystal form. The TGA diagram of the crystal form is shown in Figure 7 As shown, the DSC diagram is shown in Figure 9 shown. The upper curve in the TGA diagram is based on the right ordinate, and the lower curve is based on the left ordinate.
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Embodiment 2
[0042] Add 4.00 g of lornoxicam solids and 60 g of acetone into a four-necked reaction flask, start stirring, start heating after stirring and mixing, and control the temperature at 15° C. Add 5 wt.% triethylamine aqueous solution to adjust the pH value to 9, and the reaction system dissolves After clearing, continue stirring at 35°C for 30 minutes. Slowly add 10wt.% acetic acid aqueous solution to the clarified solution to adjust the PH<5 of the solution, and yellow crystals are precipitated, kept stirring at 35°C for 30 minutes; the solid filter cake is collected by suction filtration under reduced pressure, and the solid filter cake is placed in vacuum drying In the box, turn on the vacuum pump to evacuate (-0.07MPa~-0.1MPa), vacuum dry at 100°C for 7 hours, then cool down to 35°C, vent the nitrogen, collect the solid to obtain the solid powder of lornoxicam crystal form, Yield 98.7%, purity 99.8%.
Embodiment 3
[0044]Add 4.00g of lornoxicam solids and 64g of acetone into a four-necked reaction flask, start stirring, start heating after stirring and mixing, and add 5wt.% potassium hydroxide aqueous solution and 5wt.% N,N-di The pH value of the aqueous solution of isopropylethylamine was adjusted to 8, the reaction system was dissolved, and stirring was continued at 25° C. for 35 minutes after dissolution. Slowly add 10wt.% acetic acid aqueous solution to the clarified solution to adjust the pH<5 of the solution, and yellow crystals are precipitated, kept stirring at 25°C for 35 minutes; the solid filter cake is collected by vacuum filtration, and the solid filter cake is vacuum-dried In the box, turn on the vacuum pump to evacuate (-0.07MPa~-0.1MPa), vacuum dry at 90°C for 8 hours, then cool down to 25°C, vent the nitrogen, and collect the solid to obtain the solid powder of lornoxicam crystal form. Yield 98.5%, purity 99.7%.
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