Trifluoroacetyl substituted hydrazone derivative and synthesis method thereof
A technique for the synthesis of trifluoroacetyl groups, which is applied in the field of trifluoroacetyl substituted hydrazone derivatives and their synthesis, can solve problems such as blanks, and achieve the effects of simple operation, mild reaction conditions, and high product yields
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Embodiment 1
[0029] In a 25ml reaction flask, add 0.2mmol of p-methoxyphenyldiazonium tetrafluoroborate, 0.3mmol of triethylenediamine, 0.3mmol of 3-phenyl-1,1,1,-trifluoro Acetone, 2 ml of acetonitrile, and the reaction system was stirred at 25°C for 0.05 hour. Add water, extract the reaction solution with ethyl acetate, remove the solvent by rotary evaporation under reduced pressure, and then separate and purify by column chromatography to obtain the target product. The column chromatography eluent used is petroleum ether: ethyl acetate with a volume ratio of 10:1 ester mixed solvent to obtain the product with a yield of 97%.
Embodiment 2
[0031] In a 25ml reaction flask, add 0.2mmol of p-methoxyphenyldiazonium tetrafluoroborate, 0.3mmol of triethylenediamine, 0.3mmol of 3-phenyl-1,1,1,-trifluoro Acetone, 2 ml of acetonitrile, and the reaction system was stirred at 25°C for 0.05 hour. Add water, extract the reaction solution with methylene chloride, remove the solvent by rotary evaporation under reduced pressure, and then separate and purify by column chromatography to obtain the target product. The column chromatography eluent used is petroleum ether:ethyl acetate in a volume ratio of 10:1 ester mixed solvent to obtain the product with a yield of 97%.
Embodiment 3
[0033] In a 25 ml reaction flask, add 0.2 mmol p-methoxyphenyldiazonium hexafluorophosphate, 0.3 mmol potassium carbonate, 0.3 mmol 3-phenyl-1,1,1,-trifluoroacetone, 2 mL of acetonitrile, and the reaction system was stirred at 25°C for 0.05 hour. Add water, extract the reaction solution with ethyl acetate, remove the solvent by rotary evaporation under reduced pressure, and then separate and purify by column chromatography to obtain the target product. The column chromatography eluent used is petroleum ether: ethyl acetate with a volume ratio of 10:1 ester mixed solvent to obtain the product with a yield of 64%.
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