Novel crystal form of nilotinib

[0017] The first step is to dissolve 14g nilotinib in 100ml ethyl acetate to prepare a solution with a concentration of 0.14g / ml;

[0018] Step 2 Add 1g of activated carbon to the solution in the first step, stir, add 10ml of absolute ethanol, and filter;

[0019] The third step is to cool the filtrate obtained in the second step to -20°C and maintain it, and add 140ml of 50% ethanol aqueous solution under stirring; the stirring speed is 300 rpm, and the rate of adding ethanol aqueous solution is 8ml / min. After the addition is completed, continue Stir for 4 hours;

[0020] The fourth step is to filter, wash the filter cake with 50% ethanol aqueous solution, and dry to obtain nilotinib high-quality goods. The HPLC detection purity is 99.42%, the yield is 92.08%, and the D90 is 38.6 microns. The X-ray powder diffraction pattern is shown in the appendix figure 1 .

[0022] The first step is to dissolve 22g nilotinib in 100ml ethyl acetate; prepare a solution with a concentration of 0.22g / ml;

[0023] Step 2 Add 1g of activated carbon to the solution in the first step, stir, add 10ml of absolute ethanol, and filter;

[0024] In the third step, the filtrate obtained in the second step is cooled to -15°C and maintained, and 250ml of 60% ethanol aqueous solution is added under stirring; the stirring speed is 380 rpm, and the rate of adding ethanol aqueous solution is 12ml / min. After the addition is completed, Continue stirring for 6 hours;

[0025] The fourth step is to filter, wash the filter cake with 60% ethanol aqueous solution, and dry to obtain nilotinib high-quality goods. The HPLC detection purity is 99.78%, the yield is 92.39%, and the D90 is 24.82 microns. The X-ray powder diffraction pattern is shown in the appendix figure 1 .

[0027] The first step is to dissolve 18g nilotinib in 100ml ethyl acetate; the preparation concentration is 0.18g / ml solution;

[0028] Step 2 Add 1g of activated carbon to the solution in the first step, stir, add 10ml of absolute ethanol, and filter;

[0029] In the third step, the filtrate obtained in the second step is cooled to -18°C and maintained, and 200ml of 55% ethanol aqueous solution is added under stirring; the stirring speed is 348 rpm, and the rate of adding ethanol aqueous solution is 10ml / min. After the addition is completed, Continue stirring for 5 hours;

[0030] The fourth step is to filter, wash the filter cake with 55% ethanol aqueous solution, and dry to obtain nilotinib fine product. The HPLC detection purity is 99.88%, the yield is 93.48%, and the D90 is 30.21 microns. The X-ray powder diffraction pattern is shown in the appendix figure 1 .