1,3,4-hiadiazine derivatives as well as preparation method and application thereof
A technology of thiadiazine and derivatives, which is applied in the field of antiviral drugs to achieve superior inhibitory effects
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Embodiment 12
[0034]Preparation of Example 12-anilino-5-(1-phthalimidoethyl)-6H-1,3,4-thiadiazine (T1)
[0035]
[0036] 1-a: 2-phthalimide propionic acid Put 5.00g (33.8mmol) of phthalic anhydride, 3.60g (40.4mmol) of alanine, and 20mL of glacial acetic acid into a 50mL reaction bottle, and reflux until no raw materials The rest was left to cool, poured into 50 mL of cold water, and a white solid was precipitated, filtered, washed with water, and dried to obtain 6.50 g of a white solid, with a yield of 87.8%.
[0037] 1 HNMR (300M, DMSO-d 6 ): δ1.54(d, 3H), 4.86(q, 1H), 7.84-7.91(m, 4H), 13.11(s, 1H).
[0038] 1-b: 1-bromo-3-phthalimide-2-butanone Put 2.19g (10.0mmol) of 2-phthalimide propionic acid and 10mL of thionyl chloride in a 50mL reaction bottle, and reflux to There was no raw material left, and it was spin-dried under reduced pressure to obtain a brown oil, which was set aside. Add 15mL of 50% KOH aqueous solution into 40mL of diethyl ether, place it in an ice bath, slowly ...
Embodiment 2
[0042] Example 2 Preparation of 2-(4-fluoro-anilino)-5-(1-phthalimidoethyl)-6H-1,3,4-thiadiazine (T2)
[0043]
[0044] 0.296g (1.00mmol) of 1-bromo-3-phthalimide-2-butanone, 0.185g (1.00mmol) of 4-(4-fluoro-phenyl)-3-thiosemicarbazide, NaHCO 3 0.084g (1.00mmol), 15mL of ethanol, placed in a 50mL reaction bottle, refluxed until no raw materials remained, allowed to cool, poured into 15mL of cold water, filtered, washed with water, and dried. The resulting solid was recrystallized through 95% ethanol / DMF to obtain 0.170 g of a white solid with a yield of 44.5%.
[0045] 1 HNMR (300M, DMSO-d 6 ): δ1.65(d, 3H), 3.45(s, 2H), 5.13(q, 1H), 6.79(s, 1H), 7.08(dd, 2H), 7.83-7.90(m, 4H), 10.98( s, 1H).
Embodiment 3
[0046] Example 3 Preparation of 2-(4-chloro-anilino)-5-(1-phthalimidoethyl)-6H-1,3,4-thiadiazine (T3)
[0047]
[0048] 0.296g (1.00mmol) of 1-bromo-3-phthalimide-2-butanone, 0.201g (1.00mmol) of 4-(4-fluoro-phenyl)-3-thiosemicarbazide, NaHCO 3 0.084g (1.00mmol), 15mL of ethanol, placed in a 50mL reaction bottle, refluxed until no raw materials remained, allowed to cool, poured into 15mL of cold water, filtered, washed with water, and dried. The resulting solid was recrystallized through 95% ethanol / DMF to obtain 0.300 g of a white solid with a yield of 65.3%.
[0049] 1 HNMR (300M, DMSO-d 6 ): δ1.66(d, 3H), 3.47(s, 2H), 5.14(q, 1H), 6.79(s, 1H), 7.29(d, 2H), 7.83-7.90(m, 4H), 11.05( s, 1H).
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