Fexofenadine hydrochloride compound of novel crystal form and preparation method of fexofenadine hydrochloride compound
A technology of fexofenadine hydrochloride and fexofenadine, which is applied in the directions of active ingredients of heterocyclic compounds, organic chemistry, drug combination, etc. Solubility and bioavailability issues
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0027] Suspend 10 g of fexofenadine amorphous (from WO2009034582A2) in a mixed solution of 60 ml of pentanone and tetrahydrofuran (the volume ratio of pentanone to tetrahydrofuran is 5:1), heat to reflux for 5 hours, and add 10% Ethyl acetate solution of HCl, adjust the pH value of the reaction material to 2, stir at ambient temperature for 14 hours, filter, and dry the obtained solid at 80°C, then suspend the solid in acetone and heat to reflux for 5 hours, stir at room temperature, filter the obtained solid, 100-120 °C and vacuum-dried to obtain fexofenadine hydrochloride crystal form J9.2g of the present invention.
Embodiment 2
[0029] Suspend 10g of fexofenadine crystal form A (from CN100390145C) in a mixed solution of 62.5ml of pentanone and tetrahydrofuran (the volume ratio of pentanone to tetrahydrofuran is 7:1), heat to reflux for 5h, and add 10 % HCl in ethyl acetate solution, adjust the pH value of the reaction material to 2, stir at ambient temperature for 14 hours, filter, and dry the obtained solid at 80°C, then suspend the solid in acetone and heat to reflux for 5 hours, stir at room temperature, filter the obtained solid, 110°C Dry under vacuum to obtain fexofenadine hydrochloride crystal form J9.6g.
Embodiment 3
[0031] Suspend 10 g of fexofenadine crystal form A in a mixed solution of 100 ml of pentanone and tetrahydrofuran (the volume ratio of pentanone to tetrahydrofuran is 8:1), heat to reflux for 5 h, and add ethyl acetate containing 10% HCl to the solution. Ester solution, adjust the pH value of the reaction material to 2, stir at ambient temperature for 14 hours, filter, and dry the obtained solid at 80°C, then suspend the solid in acetone and heat to reflux for 5 hours, stir at room temperature, filter the obtained solid, and vacuum dry at 110°C, thereby Obtained fexofenadine hydrochloride crystal form J9.3g.
[0032] The XRPD diffraction data of fexofenadine hydrochloride crystalline form J prepared in Examples 1-3 are consistent with those in Table 2. DSC detection shows that crystalline form J has an obvious endothermic peak at 172±3°C.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 