Febuxostat imidazolium salt hydrate, and preparation method and application thereof
A technology of febuxostat salt and febuxostat, which is applied in the field of new drug salt forms, can solve the problems of reducing febuxostat bioavailability, affecting absorption, low water solubility of febuxostat, etc., and achieving rapid thermodynamics Stability, rapid dissolution, high crystallinity effect
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Embodiment 1
[0040] Step 1: Dissolve 40.00 mg of febuxostat and 20.00 mg of imidazole in 5 mL of saturated ethyl acetate aqueous solution, heat and stir for 0.5 h to obtain a saturated solution;
[0041] Step 2: Place the saturated solution obtained in step 1 in an environment of 0-35°C, let it stand, transfer the supernatant liquid to a glass test tube, seal the test tube opening with a parafilm, and pierce the parafilm with a needle for 2-4 After 15 days, colorless and transparent massive crystals began to separate out, and were filtered to obtain crystals;
[0042] Step 3: Place the crystal obtained in Step 2 in a vacuum oven at 60-70°C for 24 hours to obtain it. It is determined by single crystal diffraction to be febuxostat imidazolate hydrate, as shown in Figure 1-2 Shown; Compare the crystallographic data of febuxostat and febuxostat imidazolium salt hydrate, see Table 1 for details:
[0043] The crystallographic data comparison of febuxostat and febuxostat imidazolium salt hydrat...
Embodiment 2
[0047] Step 1: Dissolve 40.00 mg of febuxostat and 20.00 mg of imidazole in 5 mL of ethyl acetate, heat and stir for 1 hour to obtain a saturated solution;
[0048] Step 2: Place the saturated solution obtained in step 1 in an environment of 0-35°C, let it stand, transfer the supernatant liquid to a glass test tube, seal the test tube opening with a parafilm, and pierce the parafilm with a needle for 2-4 After 15 days, colorless and transparent massive crystals began to separate out, and were filtered to obtain crystals;
[0049] Step 3: Put the crystal obtained in Step 2 in a vacuum drying oven at 60-70°C for 24 hours to obtain.
Embodiment 3
[0051] Step 1: Dissolve 5.0 g of febuxostat and 2.00 g of imidazole in 50 mL of saturated ethyl acetate aqueous solution, heat and stir for 1 hour to obtain a saturated solution;
[0052] Step 2: Place the saturated solution obtained in step 1 in an environment of 0-35°C, let it stand, transfer the supernatant liquid to a glass test tube, seal the test tube opening with a parafilm, and pierce the parafilm with a needle for 2-4 After 20 days, colorless and transparent massive crystals began to separate out, and were filtered to obtain crystals;
[0053] Step 3: Place the crystal obtained in Step 2 in a vacuum oven at 60-70°C for 24 hours to obtain it. It is determined by XRD powder diffraction to be febuxostat imidazolate hydrate, as shown in image 3 , 4 and 5.
[0054] in, image 3 Among them, a refers to the actual PXRD pattern of imidazole, b refers to the actual PXRD pattern of febuxostat imidazole salt hydrate, c refers to the actual PXRD pattern of febuxostat imidazole ...
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