Polysubstituted benzo hetero aromatic ring and method for one step synthesizing polysubstituted benzo hetero aromatic ring
A synthesis method and a multi-substituted technology are applied in the field of synthesis of multi-substituted benzoheteroaromatic rings, can solve problems such as cumbersome transformation steps, and achieve the effects of simple synthesis method, good water resistance and air stability, and easy synthesis.
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Embodiment 1
[0039] Compound 1: Put 2-furyl boronic acid (50.4 mg, 0.45 mmol) and tetrakis-(triphenylphosphine) palladium (17.3 mg, 0.015 mmol) into a dry Schlenk reaction tube, fill with argon, add tetrahydrofuran (2.0 mL). After 10 minutes a stirred solution of the substrate (54.6 mg, 0.3 mmol) in THF (1.0 mL) was injected. The temperature of the reaction mixture was refluxed in an oil bath until the reaction of the raw materials was completed. After cooling to room temperature, the solvent was distilled off and separated by column chromatography (petroleum ether: ethyl acetate) to obtain a colorless liquid. Yield: 67%; 1 H NMR (300MHz, CDCl 3 ): δ7.60(d, J=2.4Hz, 1H), 7.17(s, 1H), 6.76(d, J=2.4Hz, 1H), 5.23(s, 2H), 5.18(s, 2H), 2.37 (s, 3H); 13 C NMR (75MHz, CDCl 3): δ154.9, 145.0, 135.1, 131.6, 127.1, 123.4, 104.9, 101.4, 73.7, 72.5, 15.7; MS (EI, 70eV): m / z (%): 174 (M + , 35), 159(41), 145(100), 131(23), 115(28); IR(CHCl 3 , cm -1 ): 2852(s), 1382(s), 1297(s), 1141(s), 1038(...
Embodiment 2
[0041] Compound 2: put 2-furyl boronic acid (50.4mg, 0.45mmol) and tetrakis-(triphenylphosphine) palladium (17.3mg, 0.015mmol) into the dry Schlenk reaction tube, fill with argon, add tetrahydrofuran (2.0 mL). After 10 minutes a stirred solution of the substrate (77.4 mg, 0.3 mmol) in THF (1.0 mL) was injected. The temperature of the reaction mixture was refluxed in an oil bath until the reaction of the raw materials was completed. After cooling to room temperature, the solvent was distilled off and separated by column chromatography (petroleum ether: ethyl acetate) to obtain a colorless liquid. Yield: 75%; 1 H NMR (300MHz, CDCl 3 ): δ7.58(d, J=2.1Hz, 1H), 7.29-7.13(m, 6H), 6.69(dd, J=1.2, 2.1Hz, 1H), 5.18(s, 2H), 5.04(s, 2H), 4.11(s, 2H); 13 C NMR (75MHz.CDCl 3 ): δ155.2, 145.1, 139.2, 136.4, 132.9, 128.6, 128.4, 127.1, 126.3, 126.2, 105.1102.2, 73.5, 72.3, 36.8; m + , 82), 221(38), 172(100), 159(34), 131(35), 115(47), 78(40), 51(41); IR(CHCl 3 , cm -1 ): 2849(m), 1...
Embodiment 3
[0043] Compound 3: put 2-furyl boronic acid (50.4mg, 0.45mmol) and tetrakis-(triphenylphosphine) palladium (17.3mg, 0.015mmol) into the dry Schlenk reaction tube, fill with argon, add tetrahydrofuran (2.0 mL). After 10 minutes a stirred solution of the substrate (85.8 mg, 0.3 mmol) in THF (1.0 mL) was injected. The temperature of the reaction mixture was refluxed in an oil bath until the reaction of the raw materials was completed. After cooling to room temperature, the solvent was distilled off and separated by column chromatography (petroleum ether: ethyl acetate) to obtain a colorless liquid. Yield: 63%; 1 H NMR (300MHz, CDCl 3 ): δ7.60(d, J=2.1Hz, 1H), 7.57-7.54(m, 2H), 7.50-7.45(m, 2H), 7.40-7.36(m, 1H), 6.91(d, J=2.1 Hz, 1H), 5.26(s, 2H), 5.20(s, 2H), 3.15(h, J=6.9Hz, 1H), 1.40(d, J=6.9Hz, 6H); 13 C NMR (75MHz, CDCl 3 ): δ152.9, 144.7, 134.8, 134.6, 133.4, 131.6, 129.0, 128.5, 127.7, 125.5, 117.7, 106.0, 72.9, 72.6, 31.8, 22.0; MS (EI, 70eV): m / z (%): 278(M + , 1...
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