Linezolid crystal form VI and preparation method thereof
A technology of linezolid and its crystal form, which is applied in the field of linezolid crystal form VI and its preparation, can solve the problems of crystal form A that consumes a lot of organic solvents, the purity of easily damaged products, and large power consumption, so as to ensure the drug effect, Ideal dissolution effect and mild process conditions
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Embodiment 1
[0026] Weigh 5g of linezolid crystal form A (form A disclosed in WO 2011 / 050826), add it to 75ml of water, cool down to 0°C, add 2mol / L concentrated hydrochloric acid, stir until the solid dissolves completely, and keep the internal temperature (that is, keep Solution temperature) is 0°C, dropwise add potassium hydroxide aqueous solution with a mass percentage concentration of 20%, adjust PH=7, continue to heat and stir for 30 minutes, filter, wash the solid with water until neutral, and dry Delineate under reduced pressure at 40°C Azolamide crystal form VI 4.81g.
[0027] The crystal form VI of linezolid obtained in this example, the X-ray powder diffraction pattern of linezolid crystal form VI is as follows: figure 1 (The abscissa is the 2-theta angle (°), the ordinate is the relative intensity (%), and the number marked in the figure is the interplanar distance (?)). The X-ray powder diffraction pattern data are shown in the following table:
[0028] Relative Stre...
Embodiment 2
[0031] Weigh 5g of linezolid crystal form II (form II disclosed in EP1255754), add it to 25ml of water, add 3mol / L formic acid, stir until the solid dissolves completely, keep the internal temperature at 5°C, and dropwise add 32% (mass %) sodium hydroxide aqueous solution, adjust PH=12, continue to stir for 30 minutes, filter, wash the solid with water until neutral, and dry under reduced pressure at 50°C to obtain 4.77g of linezolid crystalline form VI.
Embodiment 3
[0033] Weigh 5g of linezolid crystal form III (form III disclosed in EP2100884), add it to 40ml of water, add acetic acid, stir until the solid dissolves completely, add 50% potassium carbonate aqueous solution to it dropwise at room temperature, adjust the pH=10, continue Stir for 30 minutes, filter, wash the solid with water until neutral, and dry under reduced pressure at 40°C to obtain 4.72 g of Linezolid Form VI.
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