Synthesis method of dihydro-pyrazole sulfonamide derivatives of salicylaldehydes and application of dihydro-pyrazole sulfonamide derivatives to preparation of anticancer drugs
A technology of dihydropyrazole sulfonamide and salicylaldehyde, which is applied in the fields of drug combination, antineoplastic drugs, organic chemistry, etc., and can solve the problems of easy drug resistance, limited application range, adverse reactions, etc.
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Embodiment 1
[0013] Example 1: Preparation of 4-(5-(2-hydroxyphenyl)-3-phenyl-4,5-dihydropyrazole)benzenesulfonamide (Compound 27)
[0014]
[0015] Under stirring, chalcone (1.0g, 4.46mmol), ethanol (25mL), p-hydrazinobenzenesulfonamide (0.97g, 5.03mmol), and acetic acid (1.0mL) were added to a 50mL round bottom flask. Some solids are insoluble; transfer the flask to an oil bath, reflux the reaction for 6 hours, and follow the reaction by TLC (developer V AcOEt : V Masami alkyl =1:2). After the reaction is completed, filter, wash the solid with distilled water, and finally vacuum dry. The obtained solid is dissolved in absolute ethanol and recrystallized and purified to obtain the crystalline target compound.
[0016] Yellow crystals, the yield is 41.15%.m.p.266~268℃; 1 H NMR (DMSO-d6, 400MHz) δ: 9.95 (s, 1H, OH), 7.79~6.68 (m, 15H, ArH and NH) 2 ), 5.72(dd,J 1 =5.1, J 2 =5.1Hz, 1H, 5-H), 3.95(dd, J 1 =12.2, J 2 =12.1Hz, 1H, 4-H b ), 3.13(dd,J 1 =5.2, J 2 =5.1Hz, 1H, 4-H a ).
Embodiment 2
[0017] Example 2: Preparation of 4-(3-(2-chlorophenyl)-5-(2-hydroxyphenyl)-4,5-dihydropyrazole)benzenesulfonamide (Compound 28)
[0018]
[0019] The preparation method is the same as in Example 1.
[0020] Yellow crystals, the yield is 63.5%.m.p.220~222℃; 1 H NMR (DMSO-d6, 400MHz) δ: 9.93 (s, 1H, OH), 7.80~6.71 (m, 14H, ArH and NH2), 5.73 (dd, J 1 =5.1, J 2 =5.1Hz, 1H, 5-H), 4.09 (dd, J 1 =12.2, J 2 =12.1Hz, 1H, 4-H b ), 3.22(dd,J 1 =5.2, J 2 =5.1Hz, 1H, 4-H a ).
Embodiment 3
[0021] Example 3: Preparation of 4-(3-(4-ethoxyphenyl)-5-(2-hydroxyphenyl)-4,5-dihydropyrazole)benzenesulfonamide (Compound 29)
[0022]
[0023] The preparation method is the same as in Example 1.
[0024] White crystals, the yield is 39.5%.m.p.243~245℃; 1 H NMR (DMSO-d6, 400MHz) δ: 9.94 (s, 1H, OH), 7.72~6.68 (m, 14H, ArH and NH) 2 ), 5.67(dd, J 1 =4.9, J 2 =6.1Hz, 1H, 5-H), 4.06 (m, 2H, OCH 2 ), 3.92(dd,J 1 =12.1, J 2 =12.0Hz, 1H, 4-H b ), 3.08(dd, J 1 =6.9, J 2 =5.0Hz, 1H, 4-H a ), 1.34(t, J=6.9Hz, 3H, CH 3 ).
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