Polymorphic substance of type 5 phosphodiesterase inhibitor, and preparation method and application thereof
A type of phosphodiesterase and phosphodiesterase technology, applied in the field of medicine, can solve the problems of bioavailability to be improved, burden on patients, and low solubility
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Embodiment 1
[0125] 1. Selection of solvent: According to the solubility of the compound of formula I, the compound of formula I is insoluble at room temperature in methanol, acetonitrile and acetone, and has better solubility in tetrahydrofuran. The following 8 solvents and combinations are screened out to screen out the most suitable for forming various formula I salts. solvent. The 8 solvents and combinations are: methanol, acetone, acetonitrile, tetrahydrofuran, methanol / water (v / v=9:1), acetone / water (v / v=9:1), acetonitrile / water (v / v =9:1), tetrahydrofuran / water (v / v=9:1). The results are shown in Table 1:
[0126] Table 1
[0127]
[0128] Because the compound of formula I is insoluble at room temperature in methanol, acetonitrile and acetone, and its solubility is better in tetrahydrofuran, so in the 1st, 2, 3 and 5, 6, 7 columns of table 1, the solution before the compound of formula I is mixed with acid begins to be is cloudy, while in columns 4 and 8 the solution is clea...
Embodiment 2
[0140] Embodiment 2 pharmacokinetic test
[0141]1. The purpose of this example is to give SD rats the hydrochloride of the compound of formula I and the mesylate of the compound of formula I (derived from Preparation Examples 1 and 3) by single intragastric administration (PO) respectively, before administration and Plasma was collected at 0.25, 0.5, 0.75, 1, 2, 4, 8 and 24 hours post-dose. Liquid chromatography tandem mass spectrometry (LC-MS / MS) analysis method was used to quantitatively determine the concentration of the compound of formula I in SD rat plasma. Through WinNonlin 6.4 software, the pharmacokinetic parameters were calculated according to the non-compartmental model.
[0142] 2. Instrument: liquid chromatography tandem mass spectrometer (LCMSMS-025): the chromatograph is a Shimadzu liquid chromatograph (Japan), consisting of LC-30AD binary pump, SIL-30AC autosampler, CTO-20A column temperature Box, CBM-20A system controller and CBM-20A degasser; mass spectr...
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