Crystal form III of (S)-alpha, alpha-[(2-chlorphenyl)-(4,5,6,7-thiophane[3,2-c]pyridine-5-yl)-N'-(dimethyl)methylene] acethydrazide and preparation method thereof
A technology of tetrahydrothiophene and chlorophenyl, which is applied in the field of -α, can solve problems that do not involve the crystal form of the compound of formula I, etc.
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Embodiment 1
[0052] Weigh 5.0 g of the compound of formula I, add 20 mL of acetonitrile-tetrahydrofuran mixture (volume ratio 65:35), heat to 35 ° C, stir and dissolve, keep warm for 4 hours, filter while it is hot, control the cooling rate to slowly cool to room temperature, place. A solid was precipitated, filtered, and dried in vacuum for about 24 hours to obtain a colorless crystalline powder.
Embodiment 2
[0054] Weigh 5.0 g of the compound of formula I, add 40 mL of acetonitrile-tetrahydrofuran mixture (volume ratio 70:30), heat to 45 ° C, stir and dissolve, keep warm for 8 hours, filter while hot, control the cooling rate to slowly cool to room temperature, place. A solid was precipitated, filtered, and dried in vacuum for about 24 hours to obtain a colorless crystalline powder.
Embodiment 3
[0056] Weigh 5.0 g of the compound of formula I, add 60 mL of acetonitrile-tetrahydrofuran mixture (volume ratio 80:20), heat to 60 ° C, stir and dissolve, keep warm for 12 hours, filter while hot, control the cooling rate to slowly cool to room temperature, place. A solid was precipitated, filtered, and dried in vacuum for about 24 hours to obtain a colorless crystalline powder.
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Abstract
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