A kind of synthetic method of 2,4-diaryl quinoline compound
A technology of diarylquinoline and synthetic method, which is applied in the direction of organic chemistry, and can solve the problems of long reaction time and easy self-condensation of raw materials
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Embodiment 1
[0057] The reaction formula is as follows:
[0058]
[0059] Dissolve 0.0599g 1a (0.2mmol) and 0.1082g tetrachloro-p-benzoquinone (0.44mmol) in 3mL of acetonitrile, and stir the reaction system magnetically at 80°C for 2h. After the reaction, concentrate under reduced pressure and separate through a silica gel column. Petroleum ether and ethyl acetate at a ratio of 20:1 were used as eluents, and the eluent containing the target product was collected and combined to evaporate the solvent to obtain 2a (0.0390 g) as a yellow solid with a yield of 66%. 1 H NMR (500MHz, CDCl 3 ):δ8.21-8.17(m,3H),7.80(s,1H),7.68(s,1H),7.61-7.53(m,8H),7.48(t,J=7.3Hz,1H),2.50( s,3H). 13 C NMR (126MHz, CDCl 3 ):δ156.0,148.5,147.4,139.8,138.7,136.2,131.7, 129.9,129.5,129.1,128.8,128.6,128.3,127.5,125.7,124.4,119.4,21.8.ESI m / z[M+H] + 296.1; HRMS(ESI):calcd.forC 22 h 17 N[M+H] + 296.1434; found 296.1435.
Embodiment 2
[0060] Example 2: 0.0599g 1a (0.2mmol) and 0.1000g DDQ (0.44mmol) were dissolved in 3mL of acetonitrile, and the reaction system was magnetically stirred at 80°C for 2h. After the reaction was completed, it was concentrated under reduced pressure and separated by a silica gel column. Petroleum ether and ethyl acetate at a ratio of 20:1 were used as eluents, and the eluents containing the target product were collected and combined to evaporate the solvent to obtain 2a (0.0284 g) as a yellow solid with a yield of 48%. 1 H NMR (500MHz, CDCl 3 ):δ8.21-8.17(m,3H),7.80(s,1H),7.68(s,1H),7.61-7.53(m,8H),7.48(t,J=7.3Hz,1H),2.50( s,3H). 13 C NMR (126MHz, CDCl 3 ):δ156.0,148.5,147.4,139.8,138.7,136.2,131.7, 129.9,129.5,129.1,128.8,128.6,128.3,127.5,125.7,124.4,119.4,21.8.ESI m / z[M+H] + 296.1; HRMS(ESI):calcd.forC 22 h 17 N[M+H] + 296.1434; found 296.1435.
Embodiment 3
[0061] Example 3: 0.0599g 1a (0.2mmol) and 0.1082g tetrachloro-p-benzoquinone (0.44mmol) were dissolved in 3mL of 1,4-dioxane, and the reaction system was magnetically stirred at 80°C for 2h. After the reaction, the Concentrated under reduced pressure, separated by silica gel column, using petroleum ether and ethyl acetate at a volume ratio of 20:1 as the eluent, collecting and combining the eluent containing the target product and evaporating the solvent to obtain 2a (0.0431g) as a yellow solid, The yield was 73%. 1 H NMR (500MHz, CDCl 3 ):δ8.21-8.17(m,3H),7.80(s,1H),7.68(s,1H), 7.61-7.53(m,8H),7.48(t,J=7.3Hz,1H),2.50( s,3H). 13 C NMR (126MHz, CDCl 3 ):δ156.0,148.5, 147.4,139.8,138.7,136.2,131.7,129.9,129.5,129.1,128.8,128.6,128.3,127.5,125.7,124.4,119.4,21.8. ESI m / z[M+H] + 296.1;HRMS(ESI):calcd.for C 22 h 17 N[M+H] + 296.1434; found 296.1435.
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