Electrochemical catalyzed synthesis method for acyl substituted electron-deficient nitrogen-containing heterocyclic compound
The technology of a nitrogen heterocyclic compound and its synthesis method, which is applied in the field of electrochemical catalytic synthesis, can solve the problems of poor chemical selectivity, incomplete reaction of raw materials, long reaction time, etc., and achieve reduced energy consumption, low equipment cost, and simple operation Effect
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Embodiment 1
[0032] Example 1: Synthesis under electrochemical conditions to realize the Minisci acylation reaction of α-keto acid and nitrogen-containing heterocyclic aromatic compound
[0033] In a 50 mL single-chamber electrolytic cell, quinoxaline (1.0 mmol), pyruvic acid (3.0 mmol), HFIP (2.0 mmol) and ammonium iodide (0.15 mmol) were added to 15 mL of 0.1 M lithium perchlorate In the acetonitrile solution, with the graphite sheet electrode as the anode and the graphite sheet as the cathode, at 3mA / cm 2 Electrolyze at a constant current, stir at 70°C, stop electrolysis when the current flow reaches 2.7 F / mol, remove the solvent, dissolve with dichloromethane, wash with water three times, and separate by column chromatography to obtain acetylquinoxaline. Yield: 56%.
[0034]
[0035] yellow solid; 1 H NM R (400MHz, CDCl 3 )δ2.84(s,3H),7.82-7.90(m,2H),8.14-8.19(m,2H),9.47(s,1H);
Embodiment 2
[0036] Example 2: Synthesis under electrochemical conditions to realize the Minisci acylation reaction of α-keto acid and nitrogen-containing heterocyclic aromatic compound
[0037] In a 50mL single-chamber electrolytic cell, quinoxaline (1.0mmol), pyruvic acid (3.0mmol), and ammonium bromide (0.15mmol) were added to 15mL of acetonitrile solution dissolved in 0.1M lithium perchlorate, and graphite The sheet electrode is the anode, the graphite sheet is the cathode, at 3mA / cm 2 Electrolyze at a constant current, stir at 25°C, stop electrolysis when the current flow reaches 2.7F / mol, remove the solvent, dissolve with dichloromethane, wash with water three times, and separate by column chromatography to obtain acetylquinoxaline. Yield: 5%.
Embodiment 3
[0038] Example 3: Synthesis under electrochemical conditions to realize the Minisci acylation reaction of α-keto acid and nitrogen-containing heterocyclic aromatic compound
[0039] In a 50mL single-chamber electrolytic cell, quinoxaline (1.0mmol), pyruvic acid (3.0mmol), and ammonium bromide (0.15mmol) were added to 15mL of acetonitrile solution dissolved in 0.1M lithium perchlorate, and graphite The sheet electrode is the anode, the graphite sheet is the cathode, at 3mA / cm 2 Electrolyze at a constant current, stir at 40°C, stop electrolysis when the current flow reaches 2.7 F / mol, remove the solvent, dissolve with dichloromethane, wash with water three times, and separate by column chromatography to obtain acetylquinoxaline. Yield: 17%.
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