Bishydrazide structure compound, preparation method and application thereof
A technology of compounds and hydrates, applied in the preparation of hydrazides, active ingredients of heterocyclic compounds, digestive system, etc., can solve problems such as lack of treatment methods and lack of IBD drugs
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Embodiment 1
[0167] Example 1 Compound A 1 Synthesis:
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[0169] Step 1: Dissolve compound 1 (500 mg) in DCM (10 mL), cool down to 0°C, add compound 3 (348 mg), slowly warm up to room temperature, and keep at room temperature for 30 minutes. The reaction was quenched by adding water, extracted with ethyl acetate, concentrated under reduced pressure, and the residue was purified by column chromatography using petroleum ether: ethyl acetate = 5:1 as eluent to obtain compound 2 (610 mg, yield 84%). 1 HNMR (400MHz, CDCl3): δ8.00(d, J=8.8Hz, 2H), 7.60(d, J=8.8Hz, 2H), 3.90(s, 3H), 1.53(m, 1H), 1.12(m ,2H),0.88(m,2H).
[0170] Step 2: Dissolve compound 2 (400 mg) in CH3CH2OH (25 mL), add hydrazine hydrate (5 mL), and reflux for 4 h. After the reaction was completed, it was concentrated under reduced pressure, and the solid was washed with ice water, and then recrystallized from ethanol to obtain compound 4 (120 mg, yield 40%). 1 HNMR (400MHz, CD3OD): δ7.74(d, J=9.2Hz, 2H), 7.65(d, ...
Embodiment 2
[0172] Example 2 Compound A 2 Synthesis
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[0174] Compound A 1 (100mg) and K 2 CO 3 (74mg) was dissolved in DMF (2mL), CH was added dropwise under stirring 3 I, continue stirring overnight. After the reaction was completed, the reaction was quenched with water, extracted with EA, dried with anhydrous sodium sulfate, concentrated under reduced pressure, and the residue was purified by column chromatography with petroleum ether: ethyl acetate = 5: 1 eluent to obtain compound A 2 (90 mg, 85% yield). 1 H NMR (400MHz, DMSO-d 6 ):δ10.37(s,1H),7.57(d,J=8.8Hz,1H),7.20(d,J=8.8Hz,1H),3.12(s,3H),2.94(s,1H),1.75 (m,1H),1.45(m,3H),1.19(m,2H),0.88(m,4H),0.79(d,J=5.6Hz,4H).LRMS(ESI):387.0(M) + .
Embodiment 3-37
[0175] Example 3-37 Compound A 3 -A 37 Synthesis
[0176] With reference to the method of Example 1-2, the substrate in Example 1 was replaced with the corresponding substrate, thereby synthesizing Compound A 3 -A 37 .
[0177] The structures and characterization results of compounds A3-A37 are as follows:
[0178] Table A
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