New velpatasvir intermediate crystal form
A technology of crystal forms and polymorphs, which is applied in the field of new crystal forms of velpatasvir intermediates, can solve the problems of difficult formula I compounds and poor crystallinity of formula I compounds
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preparation example Construction
[0060] The polymorphic form of the present invention can be prepared by the following preparation method, which includes the steps of: mixing the compound of formula I and an inert solvent, and placing it, so as to obtain the polymorphic form of the present invention; wherein, The inert solvent is selected from the following group: toluene, isopropyl ether or a mixed solvent of the two.
[0061] The compound of formula I may be other polymorphs or amorphous form of the compound of formula I.
[0062] In another preferred example, the purity of the compound of formula I is ≤92%.
[0063] In another preferred example, the weight and volume ratio (g / mL) of the compound of formula I to the inert solvent is 1:0.5-1:100; preferably, 1:1-1:20.
[0064] In another preferred embodiment, after the mixing, the resulting mixture is a solution or a suspension.
[0065] In another preferred example, the standing is for 8-72 hours; preferably, for 12-48 hours; more preferably, for 12-24 hour...
Embodiment 1
[0086] The preparation of embodiment 1 crystal form I
[0087] (1) Weigh 74 mg of the compound of formula I (HPLC purity: 91.6%) into a 1.5 ml centrifuge tube, and add 0.1 mL of toluene. Sonicate until dissolved. After standing at room temperature for 16 hours, a solid precipitated out. Part of the solid precipitate was taken and identified as crystal by polarizing microscope.
[0088] (2) Place the centrifuge tube in a centrifuge, centrifuge at 12,000 rpm for 5 minutes, remove the supernatant, and dry the separated solid at room temperature for 1 hour.
[0089] (3) Characterize the solid form of the dried solid by XRPD, DSC and TGA.
[0090] result
[0091] (1) XRPD pattern
[0092] The crystal of the compound of formula I is named as crystal form I, and its XRPD pattern is as follows: figure 1 shown. The main diffraction peaks and their relative intensities are shown in Table 1.
[0093] Table 1 XRPD data of the crystal
[0094] 2θ(°)
Relative Strength(...
Embodiment 2
[0102] (1) Weigh 74 mg of the compound of formula I (HPLC purity: 91.6%) into a 1.5 ml centrifuge tube, and add 0.1 mL of isopropyl ether. Sonication forms a suspension. After standing at room temperature for 16 hours, a part of the solid precipitate was taken and identified by a polarizing microscope, which was confirmed to be a crystal.
[0103] (2) Place the centrifuge tube in a centrifuge, centrifuge at 12,000 rpm for 5 minutes, remove the supernatant, and dry the separated solid at room temperature for 1 hour.
[0104] (3) Characterize the solid form of the dried solid by XRPD.
[0105] result
[0106] (1) XRPD pattern
[0107] The XRPD spectrum of the crystal obtained in Comparative Example 2 is consistent with the crystal form I XRPD spectrum, and it is confirmed to be crystal form I.
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