Flurbiprofen axetil crystal and preparation method thereof
A flurbiprofen axetil and crystal form technology, which is applied in a crystal form of flurbiprofen axetil and its preparation field, can solve the problems of cumbersome steps and high cost
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[0074] The preparation method of flurbiprofen axetil crystal form I
[0075] The present invention also provides a method for preparing flurbiprofen axetil crystal form I as described herein, specifically, the method includes:
[0076] 1. Miscible flurbiprofen axetil melt or crystals of any crystal form with a solvent.
[0077] In this step, the solvent is preferably methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, acetone, acetonitrile, tetrahydrofuran, water or a mixture thereof, more preferably methanol , isopropanol and acetone. The volume of the added organic solvent is 2 to 8 times the mass of flurbiprofen axetil.
[0078] 2. Add the seed crystals of flurbiprofen axetil to the above solution.
[0079] Wherein, the mass of the added seed crystal is preferably 0.1%-5% of the mass of flurbiprofen axetil, more preferably 0.5-2%. The seed crystal can be the ground product of flurbiprofen axetil solidified at low temperature, or the crystal o...
Embodiment 1
[0100] Charge 30g flurbiprofen axetil melt and 60mL methanol into the reactor, stir and miscible, and the solution is clear now. Add 0.3 g of flurbiprofen axetil crystal form I as a seed crystal. Stir at constant temperature at 10°C for 4h, and crystallize. Suction filter with a Buchner funnel, wash the filter cake three times with water, and freeze-dry the washed filter cake. 24g of flurbiprofen axetil crystal form I was obtained with a yield of 80% and a melting point of 35±3°C.
[0101] The obtained product is a solid white powder, and its DSC spectrum is as follows: figure 1 Shown in, result shows, this solid powder has obvious melting point in DSC collection of illustrative plates, and existing flurbiprofen axetil is colorless transparent oily liquid, prompts that the solid white powder that is prepared is crystalline form.
[0102] The obtained flurbiprofen axetil crystal form I is subjected to a powder X-ray diffraction test, and the results are as follows: figure ...
Embodiment 2
[0113] 30g of flurbiprofen axetil melt, 60mL of methanol and 180mL of purified water were charged into the reactor, stirred and miscible, and the solution was in the form of an emulsion at this time. 1.5 g of flurbiprofen axetil crystal form I was added as a seed crystal. Stir at constant temperature at 20°C for 8h to crystallize. Suction filter with a Buchner funnel, wash the filter cake three times with water, and freeze-dry the washed filter cake. 28 g of flurbiprofen axetil crystal form I was obtained with a yield of 93.3% and a melting point of 35±3°C.
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