A class of trans-diarylethenes lsd1 inhibitors, their preparation methods and applications
A technology of diarylethenes and compounds, which is applied in the field of medicinal chemistry and achieves the effects of high yield, strong LSD1 inhibitory activity and simple synthesis method
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Embodiment 1
[0026] Example 1 4-methoxy-3-(pyridin-2-yl)benzaldehyde (1a)
[0027]
[0028] Add 2-bromopyridine (456.5mg, 2.89mmol), toluene (7mL), K 2 CO 3 Aqueous solution (2.76g potassium carbonate dissolved in 10mL water, 2mL), tetrakis(triphenylphosphine)palladium (45.2mg, 0.04mmol), stirred at room temperature under nitrogen protection for 15 minutes, then added 5-formyl-2-methoxy Phenylboronic acid (400mg, 2.22mmol) in absolute ethanol (3mL), heated at 92°C for 4 hours, poured the reaction system into water, extracted with ethyl acetate, combined the ethyl acetate layers, followed by water, saturated saline Washed, dried over anhydrous sodium sulfate, suction filtered, the filtrate was concentrated under reduced pressure, and the concentrate was separated by column chromatography (petroleum ether: ethyl acetate = 6:1) to obtain 414.6 mg of white solid, yield 87.5%, Mp: 52-53 ℃. 1 H NMR (400MHz, CDCl 3 )δ9.98(s,1H),8.73(m,1H),8.31(d,1H,J=2.4Hz),7.96(dd,1H,J 1 = 2.4 Hz,J 2 =8...
Embodiment 2
[0029] Example 2 4-methoxy-3-(4-fluoropyridin-2-yl)benzaldehyde (1b)
[0030]
[0031] According to the method of Example 1, 2-bromo-4-fluoropyridine (508.6 mg, 2.89 mmol) was used instead of 2-bromopyridine to obtain 395.8 mg of white solid, yield 77.1%, Mp: 73-74°C.1 H NMR (400MHz, CDCl 3 )δ 10.00(s,1H),8.72(dd,1H,J 1 =5.6Hz,J 2 =8.8Hz),8.40(t,1H,J=2.0Hz),8.00(dd,1H,J 1 =1.2Hz,J 2 =8.8Hz),7.65(d,1H,J=10.4Hz),7.16(d,1H,J=8.4Hz),7.05(m,1H),4.01(s,3H). 13 C NMR (101MHz, CDCl 3 )δ190.88,175.95,169.87,167.27, 161.69,157.37,157.29,151.61,151.54,134.23,131.67,130.04,128.13,128.10, 113.06,112.87,111.74,110.42,110.25,56.11.HRMS(ESI)calcd for C 13 h 10 FNNaO 2 [M+Na] + :254.0588,Found:254.0582.
Embodiment 3
[0032] Example 3 4-methoxy-3-(pyrimidin-2-yl)benzaldehyde (1c)
[0033]
[0034] According to the method of Example 1, 2-bromopyridine was replaced with 2-bromopyrimidine (445.1 mg, 2.80 mmol) to obtain 414.2 mg of white solid, yield 87.1%, Mp: 80-81°C. 1 H NMR (400MHz, CDCl 3 )δ 9.96(s,1H),8.88(d,2H,J=4.8Hz),8.26(d,1H,J=2.4Hz),8.00(dd,1H,J 1 = 2.4 Hz,J 2 =8.8Hz),7.29(t,1H,J=4.8Hz),7.16(d,1H,J=8.8Hz),3.96(s,3H). 13 C NMR (101MHz, CDCl 3 )δ190.61, 164.71, 162.41, 157.17, 134.47, 132.52, 129.64, 128.77, 119.23, 112.05, 56.44. HRMS (ESI) calcdfor C 12 h 10 N 2 NaO 2 [M+Na] + : 237.0634,Found: 237.0639.
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