Tizanidine hydrochloride compound
A technology for tizanidine hydrochloride and a compound, which is applied in the field of preparation of the compound crystal I, can solve the problems that the quality of the finished product is difficult to meet the standard, difficult to remove colored impurities, and there are many impurities in tizanidine hydrochloride, so as to achieve stable properties and improve biological performance. Availability and safety, good water solubility
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Embodiment 1
[0033] The preparation of embodiment 1 tizanidine hydrochloride compound
[0034] Weigh 50g of tizanidine hydrochloride, add a mixed solution of 125mL ethanol and 125mL water, heat up to 75°C, after the dissolution is complete, add an appropriate amount of activated carbon, filter while hot, and slowly cool the filtrate to room temperature at 0.5°C / min, continue Stir for 1 hour, then stand at room temperature for 8 hours, filter with suction, wash, and dry to obtain 49.1 g of tizanidine hydrochloride compound crystal I in the form of white powder, with a yield of 98.2%. Mass spectrum showed its ESI m / z: 254.
[0035] The measured melting point of tizazidine hydrochloride compound crystal I is 285.0-286.5°C. Using CuKα radiation, the X-ray powder diffraction pattern of tizanidine hydrochloride compound crystal I is measured in figure 1 , and the diffraction related data are shown in Table 1 (2θ measurement error is ±0.2).
Embodiment 2
[0038] The preparation of embodiment 2 tizanidine hydrochloride compound
[0039] Weigh 50g of tizanidine hydrochloride, add a mixed solution of 350mL ethanol and 50mL water, heat up to 50°C, after the dissolution is complete, add an appropriate amount of activated carbon, filter while hot, and slowly cool the filtrate to room temperature at 0.5°C / min, continue Stir for 0.5 hour, then stand at room temperature for 24 hours, filter with suction, wash, and dry to obtain 48.4 g of crystal I of tizanidine hydrochloride compound in the form of white powder, with a yield of 96.8%. The structural analysis results and X-ray powder diffraction patterns of the obtained product are not significantly different from those in Example 1.
Embodiment 3
[0040] The preparation of embodiment 3 tizanidine hydrochloride compound
[0041]Weigh 50g of tizanidine hydrochloride, add a mixed solution of 690mL ethanol and 60mL water, heat up to reflux, after the dissolution is complete, add an appropriate amount of activated carbon, filter while hot, and slowly cool the filtrate to room temperature at 0.8°C / min, then continue to stir After 2.5 hours, it was allowed to stand at room temperature for 16 hours, filtered with suction, washed, and dried to obtain 48.5 g of crystals of tizanidine hydrochloride compound I in the form of white powder, with a yield of 97.0%. The structural analysis results and X-ray powder diffraction patterns of the obtained product are not significantly different from those in Example 1.
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