A kind of crystallization preparation method of small particle size febuxostat
A technology of febuxostat and crystallization, which is applied in the field of crystallization preparation of small particle size febuxostat, can solve problems such as difficulty in obtaining products with required particle size distribution, a large amount of waste and dust pollution, poor ability to control particle size, etc., to achieve Avoid the effects of high energy cost, good fluidity, and easy industrial production
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Embodiment 1
[0036] Put 10 g of febuxostat into 210 ml of 98% butanone aqueous solution, and continuously stir and dissolve at 65 °C for 30 min; filter while it is still hot; transfer the filtrate into a crystallizer and stir at a constant temperature of 65 °C, and then heat at 6 min / min. The cooling rate was lowered to 40°C, and 0.05 g of seed crystals were added at the end of cooling, and the crystals were incubated at constant temperature for 1 h. The system was re-heated to 50 °C, the heating rate was 2 min / °C, and the crystal was incubated at a constant temperature for 2 h at the end of the heating. Cool the system again to 20°C at a rate of 3 min / °C, and cultivate the crystals at a constant temperature for 2 h at the end of the cooling. The system was heated up again, raised to 35°C at a rate of 6 min / °C, and then cooled to 0°C at a rate of 3 min / °C after culturing for 2 hours. Dry at 70 °C at atmospheric pressure for 8 h. The yield of the final product is 89.1%, the HPLC purity is...
Embodiment 2
[0038] Put 10 g of febuxostat into 210 ml of 90% methyl ethyl ketone aqueous solution, and continuously stir and dissolve at 72 °C for 30 min; filter while it is still hot; transfer the filtrate into a crystallizer and stir at a constant temperature of 72 °C, and then stir at a constant temperature of 8 min / °C. The cooling rate was lowered to 45 °C, and 0.05 g of seed crystals were added at the end of cooling, and the crystals were incubated at a constant temperature for 1 h. The system was reheated to 55°C with a heating rate of 4 min / °C. At the end of the temperature rise, the crystals were incubated at a constant temperature for 1 h. Then the cooling system was lowered to 20°C, and the cooling rate was 5 min / °C. At the end of cooling, the crystals were incubated at a constant temperature for 3 h. The system was heated up to 35°C again at a heating rate of 4 min / °C, and after culturing for 1 h, the temperature was lowered to 5°C again at a rate of 4 min / °C. After dropping...
Embodiment 3
[0040]Put 10 g of febuxostat into 140 ml of 99% butanone aqueous solution, and continuously stir and dissolve for 30 min at a reflux temperature of 79 °C; filter while it is still hot; transfer the filtrate into a crystallizer and stir at a constant temperature of 79 °C, and then use Cool the system to 50°C at a cooling rate of 2 min / °C, add 0.10 g of seed crystals at the end of cooling, and then keep the crystals at constant temperature for 2 h. The system was re-heated to 65 °C, the heating rate was 3 min / °C, and the temperature was kept constant for 3 h at the end of the heating, and then the system was cooled to 25 °C, the cooling rate was 6 min / °C, and the crystal was incubated at the end of the cooling for 1 h. The system was heated up to 40°C again at a heating rate of 2 min / °C, and after culturing for 1 h, the temperature was lowered to 10°C again at a rate of 6 min / °C. After dropping to the target temperature, it was directly filtered, and the filter cake was washed w...
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