The preparation method of palbociclib crystal form b
A technology of palbocicini crystal and crystal form, which is applied in the field of preparation of palbociclib crystal form B, can solve the problems that do not involve the preparation method of crystal form B, and achieve the effect of improving purity and simple preparation process
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[0024] The preparation of palbociclib organic acid salt or inorganic acid salt is prepared according to common technical means in this field, such as the preparation method of palbociclib hydrochloride is:
[0025] Dissolve 190g of palbociclib in 2.5L of methanol, add dropwise 360ml of 6mol / L hydrochloric acid, heat for reaction, after the reaction is completed, cool down and crystallize to obtain palbociclib hydrochloride, filter, and dry to obtain 176g of palbociclib hydrochloride .
[0026] For example, the preparation method of palbociclib isethionate is:
[0027] Dissolve palbociclib in methanol, add isethionic acid methanol solution, heat for reaction, after the reaction is completed, cool down and crystallize to obtain palbociclib isethionate.
Embodiment 1
[0029] Add 176 g of palbociclib hydrochloride to 5 L of purified water, heat to 55°C and stir for 1.5 hours, then cool down to 30°C to obtain solution ①;
[0030] Drop the solution ① into ammonia water pre-cooled to -5°C (0.7kg of ammonia water with a content of 25% to 28% is dissolved in 8L of purified water). Stir at 5-0°C for 4 hours; filter, wash the filter cake with 1 L of purified water and 1 L of acetone in turn, and dry the filter cake in vacuum for 24 hours to obtain 160 g of palbociclib in crystal form B with a yield of 84.2%. The X-ray diffraction pattern is as follows: figure 2 , the measured specific surface area is 6.8m 2 / g, HPLC purity 99.91%.
Embodiment 2
[0032] Add 88 g of palbociclib hydrochloride to 2.5 L of purified water, heat to 55°C and stir for 1.5 hours, then cool down to 20°C to obtain solution ①;
[0033] Drop solution ① into ammonia water at 30°C (dissolve 0.4kg of ammonia water with a content of 25% to 28% in 4L of purified water), control the temperature at 25 to 35°C during the dropping process, and stir at 25 to 35°C after dropping 4 hours; filter, the filter cake was washed successively with 0.5L of purified water and 0.5L of acetone, and the filter cake was vacuum-dried for 24 hours to obtain 76g of crystalline form A palbociclib, and the X-ray diffraction pattern was as follows: figure 1 , HPLC purity 99.83%.
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