A kind of tolfaminic acid-piperazine salt type and preparation method thereof
A technology of tolfenac and piperazine, applied in salt form and preparation thereof, in the field of tolfenac, and can solve problems such as low solubility of tolfenac
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Embodiment 1
[0034] Accurately weigh 724mg of tolfaminic acid and 155mg of piperazine, place them in a 50ml crystallizer, add 35g of methanol to it, heat to 30°C, and stir to dissolve the solid part to form a suspension. Keep the temperature constant at 30°C and continue to stir to carry out reaction crystallization. After continuous stirring for 12 hours, the obtained solid was filtered while it was hot, washed with mother liquor, and dried at 25° C. under normal pressure for 6 hours.
[0035] The powder X-ray diffraction pattern of the product has characteristic peaks at 2θ of 9.7, 13.9, 18.6, 23.3, 25.0, 25.3, 26.4, 26.6, 28.6, 29.2, 32.9, and 33.1 degrees. DSC shows that its melting point is 200.65 ° C, confirming the obtained The solid is in the form of tolfane acid-piperazine salt. In the water-ethanol mixed solvent with a volume ratio of 1:1, the concentration of trofenamic acid in the saturated solution at 37°C was measured to be 1.28mg / ml, while the solubility of trofenamic acid ...
Embodiment 2
[0037] Accurately weigh 745mg of tolfaminic acid and 155mg of piperazine, place them in a 50ml crystallizer, add 54g of methanol to it, heat to 20°C, and stir to dissolve the solid part to form a suspension. Keep the temperature constant at 20°C and continue to stir to carry out reaction crystallization. After continuous stirring for 12 hours, the obtained solid was filtered while it was hot, washed with mother liquor, and dried at 25° C. under normal pressure for 8 hours.
[0038] The powder X-ray diffraction pattern of the product has characteristic peaks at 2θ of 9.6, 13.9, 18.6, 23.3, 25.0, 25.3, 26.4, 26.6, 28.6, 29.1, 32.9, and 33.0 degrees. DSC shows that its melting point is 201.92 ° C, confirming the obtained The solid is in the form of tolfane acid-piperazine salt. In the water-ethanol mixed solvent with a volume ratio of 1:1, the concentration of trofenamic acid in the saturated solution at 37°C was measured to be 1.29mg / ml, while the solubility of trofenamic acid ...
Embodiment 3
[0040]Accurately weigh 930 mg of tolfaminic acid and 155 mg of piperazine, place them in a 100 ml crystallizer, add 30 g of ethanol to it, heat to 40°C, and stir to dissolve the solid part to form a suspension. Keep the temperature constant at 40°C and continue to stir to carry out reaction crystallization. After continuous stirring for 10 h, the obtained solid was filtered while it was hot, washed with mother liquor, and dried at 25° C. under normal pressure for 8 h, and the obtained product was the tolfane-piperazine salt type.
[0041] The powder X-ray diffraction pattern of the product has characteristic peaks at 2θ of 9.6, 13.9, 18.6, 23.2, 25.0, 25.3, 26.4, 26.5, 28.6, 29.2, 33.0, and 33.1 degrees. DSC shows that its melting point is 202.54 ° C, confirming the obtained The solid is in the form of tolfane acid-piperazine salt. In the water-ethanol mixed solvent with a volume ratio of 1:1, the concentration of trofenamic acid in the saturated solution at 37°C was measured...
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