Synthetic method and application of 3-cyanoimidazo[1,2-a]pyridine compound
A cyanoimidazole and synthesis method technology, applied in the field of synthesis of 3-cyanoimidazo[1,2-a]pyridine compounds, can solve the problems of lengthy reaction steps and low reaction yield, and achieve simple operation, The effect of easy to obtain and simple raw materials
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Embodiment 1
[0020]
[0021] The following steps were adopted: 2-aminopyridine (56 mg, 0.6 mmol), acetophenone (60 mg, 0.5 mmol), CuI (95 mg, 0.5 mmol) were added to a 25 mL reaction tube, NMP (1 mL) was added, and finally phenylacetonitrile was added. (70 mg, 0.6 mmol). The reaction solution was placed in an oil bath at 120° C. and reacted under air conditions for 17 hours. After the reaction was completed, the reaction mixture was cooled to room temperature, 10 mL of ethyl acetate was added to it, filtered through celite, the filtrate was poured into 15 mL of water, and extracted three times with ethyl acetate (3×5 mL). The organic phases were combined, dried over anhydrous sodium sulfate, filtered, the solvent ethyl acetate was removed by a rotary evaporator, and then separated by column chromatography to obtain 80 mg of the product with a yield of 73%. 1 HNMR (400MHz, CDCl 3 ): δ8.38(dt,J=6.8,1.2Hz,1H),8.24-8.15(m,2H),7.79(d,J=9.2Hz,1H),7.58-7.43(m,4H),7.11( td,J=6.8,0.8Hz,1H). ...
Embodiment 2
[0023]
[0024] The following steps were adopted: 2-aminopyridine (56mg, 0.6mmol), 4-methylacetophenone (67mg, 0.5mmol), CuI (95mg, 0.5mmol) were added to a 25mL reaction tube, and the solvent NMP (1mL) was added, Finally phenylacetonitrile (70 mg, 0.6 mmol) was added. The reaction solution was placed in an oil bath at 120° C. and reacted under air conditions for 17 hours. After the reaction was completed, the reaction mixture was cooled to room temperature, 10 mL of ethyl acetate was added to it, filtered through celite, the filtrate was poured into 15 mL of water, and extracted three times with ethyl acetate (3×5 mL). The organic phases were combined, dried over anhydrous sodium sulfate, filtered, the solvent ethyl acetate was removed by a rotary evaporator, and then separated by column chromatography to obtain 93 mg of the product with a yield of 80%. 1 HNMR (400MHz, CDCl 3 ): δ8.36(d,J=6.8Hz,1H),8.10(d,J=8.0Hz,2H),7.77(d,J=9.2Hz,1H),7.51–7.43(m,1H),7.33 (d, J=8.0Hz, ...
Embodiment 3
[0026]
[0027]The following steps were adopted: 2-aminopyridine (56mg, 0.6mmol), 2-methylacetophenone (67mg, 0.5mmol), CuI (95mg, 0.5mmol) were added to a 25mL reaction tube, and the solvent NMP (1mL) was added, Finally phenylacetonitrile (70 mg, 0.6 mmol) was added. The reaction solution was placed in an oil bath at 100° C., and reacted under air conditions for 15 hours. After the reaction, the reaction mixture was cooled to room temperature, 10 mL of ethyl acetate was added thereto, and filtered with diatomaceous earth, the filtrate was poured into 15 mL of water, and extracted three times with ethyl acetate (3×5 mL). The organic phases were combined, dried with anhydrous sodium sulfate, filtered, and the solvent ethyl acetate was removed with a rotary evaporator, and then separated by column chromatography to obtain 65 mg of the product with a yield of 56%. 1 HNMR (400MHz, CDCl 3 ):δ8.41(d,J=6.8Hz,1H),7.83(d,J=8.8Hz,1H),7.59(d,J=7.6Hz,1H),7.55–7.48(m,1H),7.42 –7.29(m...
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