Novel crystalline forms of anticancer compound CX1409 and preparation method and application of novel crystalline forms of anticancer compound CX1409
A technology of CX1409 and compound, which is applied in the field of two new crystal forms of anticancer compound CX1409 and its preparation, can solve problems such as no crystal form, and achieve the effect of simple preparation method, good yield and high purity
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Embodiment 1
[0054] Embodiment 1: the preparation of CX1409 crude product
[0055] The preparation of CX1409 crude product specifically comprises the following steps:
[0056] (1) Dissolve CX1409-01 (15g) in DMF (45mL), then add imidazole (5.22g), control the temperature at about 20-25°C while stirring, slowly add TESCl (6.74g), dropwise, 20 Stir at ~25°C for 0.5h. After the reaction was complete, purified water (105 mL) and DCM (150 mL) were added to separate the layers. The organic phase was washed with water (105 mL) and saturated NaCl (75 mL). The liquid was separated, and the organic phase was evaporated to dryness to obtain the crude product. Add n-hexane (150 mL) and EA (15 mL) to the crude product, stir at room temperature for 1 h, filter with suction, wash the filter cake with a small amount of n-hexane, and vacuum-dry at 40°C for 2 h to obtain 16.7 g of the product CX1409-05.
[0057] (2) Under the protection of nitrogen, control the temperature at -30°C, add NaHMDS (1.0M in ...
Embodiment 2
[0062] Example 2: Preparation of CX1409 Form A
[0063] Weigh 1.0 g of crude CX1409 (prepared in Example 1) and add it to 5 mL of ethanol, stir for 10 min, then add 6 mL of ethanol, heat to 55 ° C to dissolve until clear, and keep for 45 min; slowly drop the clear solution into Stir in 9mL of 55°C water at low speed, slowly cool down to 30°C (cooling rate: 0.5°C / min), grow crystals at constant temperature for 60 minutes, then continue to slowly cool down to 20°C (cooling rate: 0.3°C / min), grow crystals for 120 minutes The resulting crystals were collected by filtration and dried at 40° C. for 16 h under vacuum to obtain 684 mg of Form A (purity: 99.63%). The powder X-ray diffraction pattern is shown in image 3 .
Embodiment 3
[0064] Example 3: Preparation of CX1409 Form A
[0065] Weigh 1.0 g of CX1409 crude product (prepared in Example 1) and add it to 10 mL of ethanol, heat to 50 ° C to dissolve until clear, and keep for 30 min; slowly drop the clear solution into 9 mL of 50 ° C water, stir at a low speed , slowly cool down to 25°C (cooling rate is 0.5°C / min), grow crystals at constant temperature for 40 minutes, then continue to slowly cool down to 15°C (cooling rate is 0.3°C / min), grow crystals for 90 minutes; the obtained crystals are collected by filtration, and in Drying at 40°C for 16 h under vacuum conditions yielded 696 mg of Form A (purity: 99.87%), and its powder X-ray diffraction pattern is shown in image 3 .
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