Crystal form of LED 225 monophosphate and preparation method thereof
A technology of monophosphate and crystal form, which is applied in the field of chemical medicine and can solve the problems of bisphosphate transformation and other problems
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Embodiment 1
[0098] The preparation method of formula (I) compound monophosphate crystal form A:
[0099] Disperse 221.3mg of the free base of the compound of formula (I) in 6.0mL of high-purity water, then add 0.1mL of 14.6mol / L concentrated phosphoric acid, stir overnight, filter, and wash the filter cake with pure water, collect the solid, and place it at 150°C The obtained solid was determined to be Form A monophosphate salt after drying in an oven overnight.
[0100] The X-ray powder diffraction data of the crystal forms obtained in this example include but are not limited to the data shown in Table 1. Its XRPD pattern is as follows figure 1 , DSC graph as shown in figure 2 , and its TGA figure is shown in image 3 .
[0101] Table 1
[0102]
[0103]
Embodiment 2
[0105] The preparation method of formula (I) compound monophosphate crystal form A:
[0106] Disperse 20.4 mg of the compound of formula (I) in 0.6 mL of high-purity water, then add two drops of 14.6 mol / L concentrated phosphoric acid, stir overnight, centrifuge, collect the solid, place it in an oven at 100° C. Detected as monophosphate form A.
[0107] The X-ray powder diffraction data of the crystal forms obtained in this example include but are not limited to the data shown in Table 2.
[0108] Table 2
[0109]
[0110]
Embodiment 3
[0112] The preparation method of formula (I) compound monophosphate crystal form A:
[0113] 1) 1.164g of the hydrochloride of the compound of formula (I) was dissolved in 12.0mL of methanol;
[0114] 2) Dissolve 0.44g of sodium hydroxide solid in 3mL of water to form a sodium hydroxide solution;
[0115] 3) Add the sodium hydroxide solution in step 2) to the solution in step 1), and a precipitate is formed. Filter, wash the filter cake with pure water, and redisperse the resulting solid in water.
[0116] 4) Add 3.0 mL of 14.6 mol / L concentrated phosphoric acid to the solution obtained in step 3), stir overnight, filter, and wash the filter cake with pure water, collect the solid, place it in an oven at 160°C, and dry it overnight to obtain a solid It was detected as monophosphate crystal form A.
[0117] The X-ray powder diffraction data of the crystal forms obtained in this example include but are not limited to the data shown in Table 3.
[0118] table 3
[0119]
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