A method for preparing type III elvitegravir crystals
A technology of crystals and crystal forms, applied in the field of preparing type III elvitegravir crystals, can solve the problems of low yield, harsh conditions, complicated and tedious operations, etc., and achieve the effects of low cost, simple operation and short preparation period
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Embodiment 1
[0041] Add 100 g of amorphous elvitegravir raw material (HPLC purity ≥ 95%) into a mixed solvent formed by 285 mL of isopropyl acetate and 15 mL of methanol, heat to reflux, then cool to 5°C, stir for 8 hours, filter, and dry in vacuo , 95 g of white solid was obtained, the mass yield was 95%, and the HPLC purity was 99.92%.
[0042] Referring to the powder X-ray diffraction test conditions described in WO2005113508A1: Cu-Kα1 ray, 40kV tube voltage, 40mA tube current, scan speed of 5° / min, step width of 0.02°, and diffraction angle of 5 to 40° for this embodiment The obtained sample is subjected to powder X-ray diffraction test, obtained as figure 1 Powder X-ray Diffraction Spectrum shown.
[0043] Depend on figure 1 It can be seen that the elvitegravir obtained by the method of this embodiment has the powder X-ray diffraction spectrum characteristics of the type III elvitegravir crystal described in WO2005113508A1: the main diffraction peak 2θ data is: 8.54, 14.02, 15.68, 1...
Embodiment 2
[0046]Add 100 g of amorphous elvitegravir raw material (HPLC purity ≥ 95%) into a mixed solvent formed by 285 mL of isopropyl acetate and 15 mL of ethanol, heat to reflux, then cool to 0°C, stir for 3 hours, filter, and dry in vacuo , 94.5 g of white solid was obtained, the mass yield was 94.5%, and the HPLC purity was 99.89%.
[0047] Referring to the powder X-ray diffraction test conditions described in WO2005113508A1: Cu-Kα1 ray, 40kV tube voltage, 40mA tube current, scan speed of 5° / min, step width of 0.02°, and diffraction angle of 5 to 40° for this embodiment The obtained sample is subjected to powder X-ray diffraction test, and the test result is consistent with figure 1 The powder X-ray diffraction spectrum shown is consistent within the error tolerance range.
Embodiment 3
[0049] Add 100 g of amorphous elvitegravir raw material (HPLC purity ≥ 95%) into a mixed solvent formed by 270 mL of ethyl acetate and 15 mL of isopropanol, heat to reflux, then cool to 0 ° C, stir for 3 hours, filter, vacuum After drying, 93 g of white solid was obtained, the mass yield was 93%, and the HPLC purity was 99.95%.
[0050] Referring to the powder X-ray diffraction test conditions described in WO2005113508A1: Cu-Kα1 ray, 40kV tube voltage, 40mA tube current, scan speed of 5° / min, step width of 0.02°, and diffraction angle of 5 to 40° for this embodiment The obtained sample is subjected to powder X-ray diffraction test, and the test result is consistent with figure 1 The powder X-ray diffraction spectrum shown is consistent within the error tolerance range.
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Abstract
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