Crystalline state Lesinurad intermediate and preparation method thereof
A crystal form and intermediate technology, applied in the field of medicine, can solve the problems of difficult purification of the final product Lesinurad, many steps, cumbersome operation, etc., and achieve the effects of convenient storage and transportation, subsequent feeding operation, stable properties, and simple operation
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Embodiment 1
[0068] Embodiment 1: the preparation of Lesinurad intermediate II crystal
[0069] In a 100mL three-neck flask, add 10g of crude Lesinurad intermediate II (23.9mmol) and 30mL of N,N-dimethylformamide, stir at room temperature to dissolve, then add 14.5mL of 3N hydrochloric acid (43.5mmol), there are a lot of solids during stirring Precipitate, then add 200mL acetone. Cool down to 0°C and continue stirring for 1h. Suction filtration, wash the filter cake with acetone, and vacuum dry to obtain 9.35g of white solid, the yield is 93.5%, and the HPLC purity is 98.8%. The obtained solid sample is subjected to powder X-ray powder diffraction, and the detection result is a crystalline solid. The obtained spectrum is shown in attached figure 1 , and the spectral data are shown in Table 1.
[0070] Table 1 embodiment 1 gained Lesinurad intermediate II crystalline powder X-ray diffraction characteristic peak data
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[0072]
[0073] The resulting crystalline sample was ...
Embodiment 2
[0074] Embodiment 2: the preparation of Lesinurad intermediate II crystal
[0075] Add 10g of crude Lesinurad intermediate II (23.9mmol) and 50mL of ethanol to a 100mL three-necked flask, heat to 30°C, stir to dissolve, then add 3.8mL of acetic acid (66.3mmol), a large amount of solids precipitate out during stirring, then add 150mL of isopropyl Alcohol, cooled to 0 ℃, continue to stir for 2h. Suction filtration, the filter cake was washed with isopropanol, and vacuum-dried to obtain 9.09 g of white solid, the yield was 90.9%, and the HPLC purity was 98.2%. The obtained solid sample was subjected to powder X-ray powder diffraction, and the detection result was a crystalline solid. The obtained See attached figure 2 , and the spectral data are shown in Table 2.
[0076] Table 2 embodiment 2 gained Lesinurad intermediate II crystalline powder X-ray diffraction characteristic peak data
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[0078]
[0079] The resulting crystalline sample was subjected to differen...
Embodiment 3
[0080] Embodiment 3: the preparation of Lesinurad intermediate II crystal
[0081] Add 10g of crude Lesinurad intermediate II (23.9mmol) and 200mL of acetonitrile to a 500mL three-necked flask, heat to 30°C, stir to dissolve, then add 23.9mL of 2N sulfuric acid (47.8mmol), a large amount of solids precipitate out during stirring, cool down to 0°C , continue to stir for 2h. Suction filtration, wash the filter cake with acetonitrile, and vacuum dry to obtain 8.86g of white solid, the yield is 88.6%, and the HPLC purity is 98.6%. The obtained solid sample is subjected to powder X-ray powder diffraction, and the detection result is a crystalline solid. The obtained spectrum is shown in attached image 3 , and the spectral data are shown in Table 3.
[0082] Table 3 embodiment 3 gained Lesinurad intermediate II crystalline powder X-ray diffraction characteristic peak data
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[0084]
[0085] The resulting crystalline sample was subjected to differential scanning calor...
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