A method for synthesizing 2,2'-dipolybenzazole compounds
A technology for dipolybenzazole and compound, which is applied in the field of synthesizing 2,2'-dipolybenzazole compounds, can solve the problems of only 35-55% yield, limited sources, low economy, etc. The effect of high economy, wide biological activity and broad application prospects
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Embodiment 1
[0037] Synthesis of 1,1'-bis(pyrimidinyl-2-yl)-1H,1'H-2,2'-diindole
[0038]
[0039] In the reaction vessel, add indole (6mmol, 702.9mg), NaH (mass fraction 60%, 10.8mmol, 432mg), DMF solvent, and react under low temperature for 30 minutes; then add 2-chloropyrimidine (9.6mmol, 1099.488mg ), the mixture was reacted at 100°C for 24 hours, cooled to room temperature, extracted to remove the solvent, and separated by column to obtain compound 1-(pyrimidinyl-2-yl)-1H-indole reactant. Accurately weigh the 1-(pyrimidinyl-2-yl)-1H-indole reactant (0.2mmol, 39.16mg) with an electronic balance, transfer to the reaction vessel, and add AgNO to the reaction vessel 3 (0.20mmol, 33.98mg), Cu(OAc) 2(0.2mmol, 39.90mg), dropwise added toluene solvent into the reaction tube, tightened the stopper of the reaction tube to seal the reaction system, heated to 130°C, and stirred for 16h. After the reaction, the reaction solution was cooled to room temperature, and the solvent was removed unde...
Embodiment 2
[0042] Synthesis of 4,4'-dimethyl-1,1'-bis(pyrimidinyl-2-yl)-1H,1'H-2,2'-diindole.
[0043]
[0044] In the reaction vessel, add 4-methylindole (6mmol, 787.08mg), NaH (mass fraction 60%, 7.2mmol, 288mg), DMF solvent, react at low temperature for 60 minutes; then add 2-chloropyrimidine (6.6 mmol, 755.898 mg), the mixture was reacted at 130°C for 16 hours, cooled to room temperature, extracted to remove the solvent, and separated by column to obtain compound 4-methyl-1-(pyrimidinyl-2-yl)-1H-indole reaction things. Accurately weigh 4-methyl-1-(pyrimidinyl-2-yl)-1H-indole reactant (0.2mmol, 41.85mg) with an electronic balance, transfer to the reaction vessel, add AgNO to the reaction vessel 3 (0.28mmol, 47.57mg), Cu(OAc) 2 (0.3mmol, 59.85mg), dropwise added toluene solvent into the reaction tube, sealed the reaction system, heated to 110°C, and stirred for 24h. After the reaction, the reaction solution was cooled to room temperature, and the solvent was removed under vacuum ...
Embodiment 3
[0047] Synthesis of 4,4'-dibenzyloxy-1,1'-bis(pyrimidinyl-2-yl)-1H,1'H-2,2'-diindole.
[0048]
[0049] In the reaction vessel, add 4-benzyloxyindole (6mmol, 1339.68mg), NaH (mass fraction 60%, 9mmol, 360mg), DMF solvent, react under low temperature condition for 40 minutes; Then add 2-chloropyrimidine (7.2 mmol, 824.616g), the mixture was reacted at 130°C for 24 hours, cooled to room temperature, extracted to remove the solvent, and separated by column to obtain compound 4-benzyloxy-1-(pyrimidinyl-2-yl)-1H-indole Reactant. Accurately weigh 4-benzyloxy-1-(pyrimidinyl-2-yl)-1H-indole reactant (0.2mmol, 60.27mg) with an electronic balance, transfer to the reaction vessel, add AgNO to the reaction vessel 3 (0.24mmol, 40.77mg), Cu(OAc) 2 (0.2mmol, 39.90mg), dropwise added toluene solvent into the reaction tube, sealed the reaction system, heated to 130°C, and stirred for 24h. After the reaction, the reaction solution was cooled to room temperature, and the solvent was remove...
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