3-(2-aminothiazole)-7-substituted piperazine quinolone compound and its preparation method and application
A technology of aminothiazoles and compounds, applied in the field of chemical synthesis, can solve problems such as drug resistance, and achieve the effect of solving drug resistance
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Embodiment 1
[0054] Embodiment 1, the preparation of intermediate IX
[0055]
[0056] Using triethyl orthoformate as the starting material, after nucleophilic substitution and cyclization, the latter undergoes N-alkylation, bromination, and ring closure with thiourea to obtain the 3-(2-aminothiazole)quinolone intermediate, Reference "Cui, S.F.; Addla, D.; Zhou, C.H. Novel 3-Aminothiazolquinolones: Design, Synthesis, Bioactive Evaluation, SARs, and Preliminary Antibacterial Mechanism. J. Med. Chem. 2016, 59, 4488–4510." method for preparation. 5.262 g of intermediate IX are obtained, yield 84.3%; yellow powder.
Embodiment 2
[0057] Embodiment 2, the preparation of intermediate X
[0058]
[0059] Anhydrous piperazine (3.874g, 45.0mmol) was added in a 150mL round bottom flask, and after stirring for 1 hour at 100°C with 30mL N-methylpyrrolidone as a solvent, quinolone intermediate IX (4.857g, 15.0mmol) was added, and then Adjust the temperature to 130° C. and stir the reaction, trace with thin-layer chromatography until the end of the reaction, and cool to room temperature. The mixture was poured into ice water, followed by post-processing such as filtration, column chromatography, recrystallization, and drying to obtain compound X (1.193g), yield 21.3%; yellow solid; melting point: >250°C.
Embodiment 3
[0060] Embodiment 3, the preparation of intermediate VIII
[0061] The intermediates VIII-1, VIII-2, VIII-3 and VIII-4 can be obtained by N-amidation of different types of aliphatic amine compounds and chloroacetyl chloride.
[0062]
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