Setastine hydrochloride crystal form F and preparation method thereof
A technology of sstatastine hydrochloride crystal and interplanar spacing, which is applied in the fields of medicine and biology, can solve the problems such as no literature report on sstatine hydrochloride crystal form F, and achieves good solvent safety, good stability, and preparation technology. simple effect
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Embodiment 1
[0029] Embodiment 1 Preparation of Sestatastine Hydrochloride Form F
[0030] Take 1.0g of stastatine hydrochloride raw material, add 5~10ml of 50% acetone water, stir and reflux for 10 minutes, the reflux temperature is not higher than 60 oC , cool down, keep 10 oC The following crystallization, the crystallization time is not less than 10 hours, after the crystallization finishes, suction filtration separates, obtains stastatine hydrochloride solid, at 40 o C~60 oC , Under the condition of vacuum degree less than 100Pa, dry under reduced pressure for more than 20 hours, and then pulverize. In diffraction angle (2θ / o ), interplanar spacing (d / ?) and abundance ratio (I / I O ) at 5.58 (15.82, 41), 8.48 (10.41, 22), 9.76 (9.05, 33), 16.24 (5.45, 32), 16.76 (5.28, 73), 18.08 (4.90, 32) , 18.60 (4.76, 38), 21.32 (4.16, 100), 23.26 (3.82, 23), 23.8 (3.73, 48), 26.46 (3.36, 22), 27.72 (3.21, 28), 28.4 (3.14, 22) Obvious characteristic absorption peaks, see attached f...
Embodiment 2
[0031] The preparation of embodiment 2 Sestatastine hydrochloride crystal form F
[0032] Take 1.0g of Sestatastine hydrochloride raw material, add 5~10ml of 50% ethanol water, and the temperature of the water bath is not higher than 60 oC Stir to dissolve, cool and keep for 10 oC The following crystallization, the crystallization time is not less than 10 hours, after the crystallization finishes, suction filtration separates, obtains stastatine hydrochloride solid, at 40 o C~60 oC , Dry under reduced pressure for more than 20 hours under the condition of vacuum degree less than 100Pa, and then crush. Gained sitastine hydrochloride crystal form FX-diffraction spectrum, infrared spectrogram and differential scanning calorimetry figure and attached figure 1 , attached figure 2 , attached image 3 Basically the same.
Embodiment 3
[0033] Embodiment 3 Preparation of Sestatastine Hydrochloride Form F
[0034] Take 1.0g of Sestatastine Hydrochloride raw material, add water 10~20ml, 60 oC water bath dissolve, 10 oC The following crystallization, the crystallization time is not less than 10 hours, after the crystallization finishes, suction filtration separates, obtains stastatine hydrochloride solid, at 40 o C~60 oC Dry it under reduced pressure for more than 20 hours, and then crush it. Gained sitastine hydrochloride crystal form FX-diffraction spectrum, infrared spectrogram and differential scanning calorimetry figure and attached figure 1 , attached figure 2 , attached image 3 Basically the same.
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