Edaravone crystal form and preparation method thereof
A technology of edaravone and its crystal form, which is applied in the field of edaravone crystal form and its preparation, can solve the problem that the related substances are not high enough, and achieve the effect of reducing the related substances and having good water solubility
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[0020] Example 1: Preparation of edaravone
[0021] Add 30g of edaravone to 120ml of ethyl acetate-ethanol=3:2 solution, heat to reflux to dissolve all, decolorize the activated carbon for 5min, filter while hot, cool the filtrate to room temperature, filter, and use a small amount of cold ethyl acetate- Ethanol=3:2 solution washing, 40° C. air drying for 5 hours, 120 mesh sieving to obtain 21.8 g of white crystalline product, yield: 72.7%.
[0022] The powder X-diffraction pattern was measured under the following experimental conditions (attached figure 1 ):
[0023] Testing unit: Modern Analysis Center of Nanjing University
[0024] Instrument: X’TRA powder diffractometer from Swiss ARL Company
[0025] Test conditions: target type: Cu; tube pressure: 40kv; tube flow: 40mA; starting angle: 3; ending angle: 40; scanning speed: 10; number of repetitions: 1; step length: 0.02; slit: 2 / 4 / 0.5 / 0.2.
[0026] The following table shows the powder X-diffraction spectrum data of edaravone pre...
Example Embodiment
[0029] Example 2: Preparation of edaravone
[0030] Add 10g of edaravone to 50ml of ethyl acetate-ethanol=3:2 solution, heat to reflux to dissolve all, decolorize the activated carbon for 3min, filter while hot, cool the filtrate to room temperature, filter, and use a small amount of cold ethyl acetate- Ethanol=3:2 solution washing, 40° C. air drying for 5 hours, 120 mesh sieving to obtain 6.73 g of white crystalline product, yield: 67.3%. The powder X-ray diffraction pattern is the same as in Example 1.
Example Embodiment
[0031] Example 3: Preparation of edaravone
[0032] Add 15g of edaravone to 60ml of ethyl acetate-ethanol=3:2 solution, heat to reflux to dissolve all, decolorize the activated carbon for 6min, filter while hot, cool the filtrate to room temperature, filter, and use a small amount of cold ethyl acetate- Ethanol=3:2 solution washing, 40° C. air drying for 5 hours, 120 mesh sieving to obtain 10.6 g of white crystalline product, yield: 70.7%. The powder X-ray diffraction pattern is the same as in Example 1.
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