Agomelatine methanesulfonic acid complex and preparation method thereof
A technology of methanesulfonic acid and complexes, applied in the field of agomelatine methanesulfonic acid complexes and its preparation
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Embodiment 1
[0033] Stir and dissolve 10.00g agomelatine in 50mL ethyl acetate, add 3.95g methanesulfonic acid at 10°C, slowly precipitate crystals under stirring, continue stirring and lower the temperature to 0°C to complete the crystallization; filter, and dissolve the solid with acetic acid 10 mL of ethyl ester was washed twice, and dried under reduced pressure at 30°C to obtain 9.14 g of a white solid; the purity was 99.7%, and the yield was 65.5%. mp: 75.0~80.0°C. 1 H-NMR (400MHz, CDCl 3 ): δ 11.09 (b, 1H), 9.82 (s, 1H), 7.75 (d, 1H), 7.67 (d, 1H), 7.35 (s, 1H), 7.24~7.29 (m, 2H), 7.16 (d , 1H), 3.97 (s, 3H), 3.71 (b, 2H), 3.34 (b, 2H), 2.86 (s, 3H), 2.42 (s, 3H). MS: ESI + m / z = 244.1 [M+H] + , ESI - m / z = 94.93 [M-H] + .
Embodiment 2
[0035] Stir and dissolve 10.00g agomelatine in 50mL isopropyl acetate, add 3.95g methanesulfonic acid at 10°C, then stir overnight at room temperature (20°C) to precipitate crystals, cool down to 0°C to complete the crystallization complete; filtered, the solid was washed twice with 10 mL of isopropyl acetate, and dried under reduced pressure at 30°C to obtain 9.95 g of a white solid; purity 99.7%, yield: 71.3%.
Embodiment 3
[0037] Stir and dissolve 10.00g agomelatine in 10mL methanol, cool down to 0°C, add 3.95g methanesulfonic acid, stir to dissolve, add 70mL isopropyl acetate, continue to stir overnight at 0°C to complete crystallization; filter, solid Wash twice with 10 mL of isopropyl acetate, and dry under reduced pressure at 30°C to obtain 8.40 g of a white solid; purity: 99.8%, yield: 60.2%.
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