3-cyan-5-(4-pyridyl)-N-n-propyl-pyridone, its preparation method and its application
A technology of pyridyl and pyridone, applied in the field of 3-cyano-5--N-n-propyl-pyridone and its preparation, achieving the effect of great development potential
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Embodiment 1
[0022] (1) Synthesis of intermediate 3-cyano-5-(4-pyridyl)-N(1H)pyridone
[0023] Add 31.4g (0.43mol) of DMF to a 100mL three-necked flask, and slowly add 24.76g (0.16mol) of phosphorus oxychloride dropwise while stirring in an ice bath. During the process of dropping phosphorus oxychloride, the reaction is violent and the temperature rises significantly , drop POCl 3 While the temperature was kept at 10°C, POCl 3 After the dropwise addition, keep the temperature at 0-10°C, then slowly drop 5g (0.054mol) 4-methylpyridine into the three-necked flask with a constant pressure titration funnel, and keep reacting for 2 hours, the color will become darker during the reaction process, After the reaction, pour the mixture into ice water, then use 30% NaOH to neutralize the solution to neutrality, filter to remove inorganic salts, and add 9.33g (0.098mol) crushed cyanide to the filtrate at 10-15°C Acetamide, then add 13.3mL of 30% NaOH solution dropwise into the reaction tank and sti...
Embodiment 2
[0027] Dissolve 2 g (0.01 mol) of the intermediate 3-cyano-5-(4-pyridyl)-N(1H) pyridone obtained in Example 1 with 30 mL of DMF and add it to a 100 mL three-necked flask for stirring, then Add 1.34g (0.012mol) of t-BuOK to the reaction tank step by step, stir evenly, then dissolve 1.45g (0.012mol) of n-bromopropane with 20mL of DMF and drop into the reaction three-necked flask, stir at 25°C React for 6 hours. The reaction process is monitored by TCL thin-layer chromatography. After the reaction is completed, the target product is purified by silica gel column chromatography to finally obtain 3-cyano-5-(4-pyridyl)-N-n-propyl-pyridone Obtained 1 g, 45% yield.
Embodiment 3
[0029] Use 10mL of DMF to dissolve 2g (0.01mol) of 3-cyano-5-(4-pyridyl)-N(1H)pyridone in a 100mL three-necked flask and stir, then add 1.34g (0.012mol) of t -BuOK was added to the reaction tank step by step, and after stirring evenly, 1.45g (0.012mol) of n-bromopropane was dissolved in 10mL of DMF and added dropwise to the reaction three-necked flask, and stirred at 20°C for 7 hours. The reaction process is monitored by TCL thin-layer chromatography. After the reaction is completed, the target product is purified by silica gel column chromatography to finally obtain 3-cyano-5-(4-pyridyl)-N-n-propyl-pyridone Obtained 0.9 g, yield 44.0%.
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