Preparation method of agomelatine crystal form I
A technology of agomelatine and crystal form, which is applied in the field of preparation of agomelatine crystal form I, which can solve the problems of poor reproducibility and crystal form stability, and achieve stable stability, simple operation, and easy scale-up The effect of industrial production
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Embodiment 1
[0045] Add 300mg agomelatine crystal form II and 9mg (3%) PVP to 0.5g absolute ethanol, heat and stir until 55°C to dissolve. At room temperature, the above solution was added to 1.5 g of n-heptane, a white solid precipitated out, stirred at room temperature for 5 minutes, filtered, the solid was washed with a small amount of n-heptane, and vacuum-dried at 40°C to constant weight to obtain a white solid. Yield 258 mg, 86% yield. Its DSC spectrum is shown in figure 1 , XRPD pattern see figure 2 , which is consistent with the literature reports, is the crystal form I of agomelatine.
[0046] In the XRPD pattern of agomelatine crystal form I, the positions corresponding to the diffraction angle 2θ values of 10.86, 11.22, 11.90, 17.60, 18.40, 19.79, 20.60, 21.28, 21.86, 22.68, 23.08±0.2° correspond to characteristic Diffraction peaks.
Embodiment 2
[0048] Add 300mg agomelatine and 9mg (3%) PVP into 0.5g absolute ethanol, heat and stir until 55°C to dissolve. At room temperature, the above solution was added to 1.5 g of n-heptane, a white solid precipitated out, stirred at room temperature for 5 minutes, filtered, the solid was washed with a small amount of n-heptane, and vacuum-dried at 40°C to constant weight to obtain a white solid. Yield was 254 mg, 84.7% yield. Its DSC spectrum and figure 1 Similar; XRPD patterns are similar to figure 2 Similar to agomelatine crystal form I.
Embodiment 3
[0050] Add 1 g of agomelatine and 100 mg (10%) of PVP into 2 g of anhydrous methanol, heat and stir until 50° C. to dissolve. Add the above solution to 20 g of n-heptane at room temperature, and a white solid precipitates out. Stir at room temperature for 3-5 minutes, filter, wash the solid with a small amount of n-heptane, and vacuum-dry at 40°C until constant weight to obtain a white solid. Yield was 833 mg, 83.3% yield. Its DSC spectrum and figure 1 Similar; XRPD patterns are similar to figure 2 Similar to agomelatine crystal form I.
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