3-[2-(aryl propylenine)hydrazino]-ethyl benzoate compound and application thereof
A technology of ethyl benzoate, propenylidene, applied in the fields of medicinal chemistry and pharmacotherapeutics
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Embodiment 1
[0028] Preparation of 3-[2-((naphthalene-1-yl)-propenylidene)hydrazino]-benzoic acid (intermediate III-1)
[0029]
[0030] 152 mg of 3-hydrazinobenzoic acid was dissolved in 4.5 mL of absolute ethanol, 182 mg of 3-(naphthalene-1-yl)acrolein (compound II-1) was added, and refluxed for 2 hours. After the reaction was completed, after cooling to room temperature, a solid precipitated out in the solution. After suction filtration, the solid was washed with a mixed solution of ethyl acetate and petroleum ether (ethyl acetate: petroleum ether = 1:20), and dried to obtain the title compound, 252 mg of a light yellow solid, with a yield of 80%.
[0031] 1 H-NMR (400MHz, DMSO-d 6 )δ: 7.15 (dd, J 1 =16Hz,J 2=9.2Hz, 1H), 7.20-7.27(m, 1H), 7.34(d, J=4.8Hz, 2H), 7.49-7.63(m, 3H), 7.67(s, 1H), 7.73(d, J= 16Hz, 1H), 7.88(d, J=8.4Hz, 1H), 7.90-7.99(m, 3H), 8.35(d, J=8.4Hz, 1H), 10.60(s, 1H), 12.83(s, 1H ).
Embodiment 2
[0033] Preparation of 3-[2-((naphthalene-1-yl)-propenylidene)hydrazino]-benzoic acid ethyl ester (compound I-1)
[0034]
[0035] Dissolve 102 mg of 3-[2-((naphthalene-1-yl)-propenylidene)hydrazino]-benzoic acid (Intermediate III-1) in 2mL of anhydrous dichloromethane, and add 105 mg of dicyclohexylcarbodiimide, stirred for 20 minutes, then moved to room temperature, added 33 mg of 4-dimethylaminopyridine and 8 mL of absolute ethanol, and reacted at room temperature for 12 hours. After the reaction, the solvent was distilled off under reduced pressure, and the residue was separated by column chromatography to obtain 80 mg of a yellow solid (Compound I-1), with a yield of 72%.
[0036] 1 H-NMR (400MHz, DMSO-d 6 )δ: 1.33(t, J=7.2Hz, 3H), 4.32(q, J=7.2Hz, 2H), 7.14(dd, J 1 =16Hz,J 2 =9.2Hz, 1H), 7.23-7.30(m, 1H), 7.34-7.39(m, 2H), 7.50-7.64(m, 3H), 7.66(s, 1H), 7.74(d, J=16Hz, 1H ), 7.88(d, J=8.4Hz, 1H), 7.90-7.98(m, 3H), 8.35(d, J=8.4Hz, 1H), 10.63(s, 1H); MS(EI) m / z 344...
Embodiment 3
[0038] Preparation of 3-[2-((3-methoxy-4-acetoxyphenyl)-propenylidene)hydrazino]-benzoic acid ethyl ester (compound I-2)
[0039]
[0040] Except for replacing 3-(naphthalene-1-yl)acrolein with 3-(3-methoxy-4-acetoxyphenyl)acrolein, the rest of the required raw materials, reagents and preparation methods are the same as in Example 1 -2, the title compound was obtained, 14 mg of khaki solid, yield 24%.
[0041] 1 H-NMR (400MHz, DMSO-d 6 )δ: 1.33(t, J=7.2Hz, 3H), 2.26(s, 3H), 3.84(s, 3H), 4.32(q, J=7.2Hz, 2H), 6.82(d, J=16Hz, 1H ), 7.05(s, J=8.4Hz, 1H), 7.08-7.16(m, 2H), 7.18-7.23(m, 1H), 7.30-7.36(m, 2H), 7.38(s, 1H), 7.64( s, 1H), 7.75 (d, J=9.2Hz, 1H), 10.54 (s, 1H); MS (EI) m / z 382.2 (M + ).
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