Crystal form of vortioxetine hydrochloride and preparation method thereof
A technology of vortioxetine and crystal form, applied in the field of drug crystals, can solve the problems of strong corrosiveness, toxicity and intractability of hydrobromic acid, and achieve the effects of relatively low toxicity and safe application
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Embodiment 1
[0101] Example 1: Preparation of vortioxetine hydrochloride crystal form II
[0102] Take 5g (16.7mmol) of vortioxetine, add 150ml of ethanol, stir and reflux, heat up to 40°C to dissolve, and slowly add 1.65g of concentrated hydrochloric acid (concentration: 37% by weight, 16.7mmol) dropwise to the vortioxetine under stirring conditions. In the ethanol solution of vortioxetine, solids precipitated during the dropping process, stirred for 20 minutes, cooled to room temperature naturally, after stirring for 1 hour, suction filtered, placed in a vacuum drying oven (40-50°C) to dry to obtain vortioxetine Hydrochloride salt form II.
Embodiment 2
[0103] Example 2: Preparation of vortioxetine hydrochloride crystal form II
[0104] Take 5g (16.7mmol) vortioxetine, add 50ml of acetone, stir and reflux, heat up to 70°C to dissolve, and slowly add 1.65g concentrated hydrochloric acid (concentration: 37% by weight, 16.7mmol) dropwise to vortioxetine under stirring condition. In the acetone solution of oxetine, solids precipitated during the dropwise addition, stirred for 20 minutes, cooled down to room temperature naturally, after stirring for 1 hour, suction filtered, and dried in a vacuum oven (40-50°C) to obtain vortioxetine Tine hydrochloride crystal form II.
Embodiment 3
[0105] Example 3: Preparation of Vortioxetine Hydrochloride Form II
[0106] Get 10g (33.5mmol) vortioxetine, add 50ml ethyl acetate, stir and reflux, heat up to 50°C to dissolve, under stirring, slowly add 3.3g concentrated hydrochloric acid (concentration is 37% by weight, 33.5mmol) dropwise to In the acetone solution of vortioxetine, solids precipitated during the dropwise addition, stirred for 20 min, cooled to room temperature, stirred for 0.5 h, filtered with suction, and dried in a vacuum oven (40-50°C) to obtain vortioxetine Tioxetine hydrochloride crystal form II.
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