Novel crystal form of ribociclib monosuccinate and preparation method
A technology of monosuccinate and crystal form, which is applied in the field of medicine and can solve problems such as easy exceeding the standard
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Embodiment 1
[0134] Example 1: Preparation of crystal form AZT-IV
[0135] Weigh 5 mg of succinic acid and dissolve it in 1 mL of isopropanol, weigh 20 mg of compound (I) and suspend it in 1 mL of isopropanol, add dropwise the solution of succinic acid in isopropanol, filter, and vacuum-dry the filter cake at 40°C to obtain a solid . The obtained solid is the crystal form AZT-IV of the monosuccinate salt of the compound of formula (I).
[0136] Carry out XRPD test to the obtained solid, its X-ray powder diffraction pattern is as follows Figure 10 Shown; Carry out TGA test to gained solid, its spectrogram is as Figure 11 As shown, it has a weight loss of about 2.8% when heated to 100 ° C, which is a monohydrate; the resulting solid is subjected to DSC testing, and its spectrum is as follows Figure 12 As shown, the melting point is 182.7°C; 1 H-NMR test, the spectrum is basically as Figure 13 Shown, is monosuccinate.
Embodiment 2
[0137] Embodiment 2: Preparation of crystal form AZT-I
[0138] Weigh 5 mg of AZT-IV in the above Example 1, dissolve it in 1.5 mL of methanol, add 5 mL of diethyl ether dropwise, filter with suction, and dry the filter cake in vacuum at 35°C to obtain a solid, which is the monosuccinate crystal of the compound of formula (I) Type AZT-I.
[0139] Carry out XRPD test to the obtained solid, its X-ray powder diffraction pattern is as follows figure 1 Shown; Carry out TGA test to gained solid, its spectrogram is as figure 2 As shown, it has a weight loss of about 3.0% when heated to 100 ° C, which is a monohydrate; the resulting solid is subjected to DSC testing, and its spectrum is as follows image 3 As shown, the melting point is 183.0°C.
Embodiment 3
[0140] Embodiment 3: Preparation of crystal form AZT-II
[0141] Weigh 5 mg of AZT-IV in the above Example 1 and dissolve it in 1.5 mL of methanol, evaporate the methanol at room temperature to obtain a solid. The obtained solid is the monosuccinate crystal form AZT-II of the compound of formula (I).
[0142] Carry out XRPD test to the obtained solid, its X-ray powder diffraction pattern is as follows Figure 4 Shown; Carry out TGA test to gained solid, its spectrogram is as Figure 5 As shown, it has about 5.5% weight loss when heated to 100°C, which is dihydrate; DSC test is carried out on the obtained solid, and its spectrum is as follows Image 6 As shown, it has an exothermic peak at 159.2°C, and its melting point is 199.6°C.
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Abstract
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