I-type crystal of N-n-propyl-3-(4-methylphenyl)-4-(4-mesylphenyl)-2,5-dihydropyrrole-2-ketone and manufacturing method thereof
A technology of methylsulfonylphenyl and methylphenyl, which is applied in the field of crystallization of antibacterial drugs, can solve the problems of fine crystallization of products, difficult filtration, poor fluidity, etc., and achieve no reduction in drug content, easy production, good The effect of crystal stability
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Embodiment 1
[0036] N-n-propyl-3-(4-methylphenyl)-4-(4-methanesulfonylphenyl)-2,5-dihydropyrrole-2-one 10.0g (according to the patent CN1318541A disclosed (Prepared by the method) was added to ethanol (150ml), heated under reflux to dissolve, slowly cooled to crystallize, continue to crystallize to room temperature, and filter the precipitated crystals. The obtained crystals were dried under reduced pressure at room temperature overnight to obtain 8.86 g of crystals with a yield of 88.6%. The ethanol solvent residue in the obtained sample is 100ppm, and the melting point is 181.0~182.0℃ by capillary method; the X-ray diffraction spectrum of the crystalline sample is shown in figure 1 , It is type I crystal. DSC spectrum see figure 2 , There is a sharp melting endothermic peak at 183.87℃. The sample was dried under reduced pressure at 80°C for 4 hours, the melting point of the dried sample was measured by capillary method at 181.5-183.0°C, and the X-ray diffraction spectrum showed type ...
Embodiment 2
[0038] Add 10.0 g of N-n-propyl-3-(4-methylphenyl)-4-(4-methanesulfonylphenyl)-2,5-dihydropyrrole-2-one to methanol (150ml), Heat to reflux to dissolve, slowly cool to 35°C to start crystallization, continue crystallization to room temperature, and filter the precipitated crystals. The obtained crystals were dried under reduced pressure at room temperature overnight to obtain 8.3 g of crystals with a yield of 83%. The methanol solvent residue of the obtained sample is 200ppm, and the melting point is 181.0~183.0℃ measured by capillary method; the characteristic peaks of the X-ray diffraction spectrum of the crystalline sample are the same figure 1 , It is type I crystal. The DSC spectrum has a sharp melting endothermic peak at 184.0°C. Then, the sample was dried under reduced pressure at 80°C for 4 hours. The capillary method of the dried sample measured the melting point of 181.5-183.0°C, and the X-ray diffraction spectrum was type I crystal. The DSC spectrum has a sharp mel...
Embodiment 3
[0040] Add 10.0g of N-n-propyl-3-(4-methylphenyl)-4-(4-methanesulfonylphenyl)-2,5-dihydropyrrole-2-one to 50% ethanol (200ml) After heating and refluxing to dissolve, slowly cooling to crystallize, crystals begin to precipitate at 65°C, a large amount of crystals are precipitated at 60°C, crystallization is continued to room temperature, and the precipitated crystals are filtered. The obtained crystals were dried overnight under reduced pressure at 60°C to obtain 9.1 g of crystals with a yield of 91%. The obtained sample has a residual ethanol solvent of 500 ppm and contains 0.45% water. The melting point of the obtained sample is 181.0-182.0 DEG C by capillary method; the X-ray diffraction spectrum of the crystalline sample is type I crystal. The DSC spectrum has a sharp melting endothermic peak at 184.42°C. Then the sample was vacuum dried at 80°C for 4 hours, the moisture content of the dried sample was 0.20%, the melting point measured by capillary method was 181.0-182.5°C...
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