Electrochemical organic reaction setup and methods
a technology of electrochemical organic and reaction setup, applied in the direction of electrolytic organic production, electrolysis components, electrolysis coatings, etc., can solve the problems of affecting the final purity of the produ
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example-1
on of 2-phenyl-1H-benzo[d]imidazole (S1)
[0059]
[0060]A 20 mL screw capped vial with a septum was equipped with the carbon pencil lead inserted as anode and aluminium cathode. Further the electrodes were connected to a 9V ordinary battery, capable of supplying constant current of 5 mA / cm2 for the electrochemical reaction. To the reaction vial was charged with benzene-1,2-diamine (0.91 mmol) and benzaldehyde (0.91 mmol) in 10 mL of methanol. The reaction mixture was stirred for 5 minutes at room temperature, followed by the addition of tetrabutylammonium iodide (TBAI) (0.047 mmole); and stirred gently at room temperature. The reaction setup cell was equipped with carbon as anode and aluminum as cathode and the mixture was electrolyzed at a constant current of ˜5 mA / cm2 at room temperature while stirring for 6 h. The progress of the reaction was monitored by TLC, after the completion of the reaction, the solvent was removed in vacuo and the crude material was purified by flash chromatog...
example-2
on of 2-(4-chlorophenyl)-1H-benzo[d]imidazole (S2)
[0061]
[0062]A 20 mL screw capped vial with a septum was equipped with the carbon pencil lead inserted as anode and aluminium cathode. Further the electrodes were connected to a 9V ordinary battery, capable of supplying constant current of ˜5 mA / cm2 for the electrochemical reaction.
[0063]To the reaction vial was charged with benzene-1,2-diamine (0.91 mmol) and 4-chlorobenzaldehyde (0.91 mmol) in 10 mL of methanol. The reaction mixture was stirred for 5 minutes at room temperature, followed by the addition of tetrabutylammonium iodide (TBAI) (0.047 mmole); and stirred gently at room temperature. The reaction setup cell was equipped with carbon as anode and aluminum as cathode and the mixture was electrolyzed at a constant current of ˜5 mA / cm2 at room temperature while stirring for 6 h. The progress of the reaction was monitored by TLC, after the completion of the reaction, the solvent was removed in vacuo and the crude material was pur...
example-3
on of 2-(1H-indol-6-yl)-1H-benzo[d]imidazole (S10)
[0064]
[0065]A 20 mL screw capped vial with a septum was equipped with the carbon pencil lead inserted as anode and aluminium cathode. Further the electrodes were connected to a 9V ordinary battery, capable of supplying constant current of ˜5 mA / cm2 for the electrochemical reaction. To the reaction vial was charged with benzene-1,2-diamine (0.91 mmol) and 6-Formylindole (0.91 mmol) in 10 mL of methanol. The reaction mixture was stirred for 5 minutes at room temperature, followed by the addition of tetrabutylammonium iodide (TBAI) (0.047 mmole); and stirred gently at room temperature. The reaction setup cell was equipped with carbon as anode and aluminum as cathode and the mixture was electrolyzed at a constant current of ˜5 mA / cm2 at room temperature while stirring for 6 h. The progress of the reaction was monitored by TLC, after the completion of the reaction, the solvent was removed in vacuo and the crude material was purified by fl...
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