A kind of method for preparing fluorine-containing secondary amine
A fluorine-containing secondary amine and primary amine technology is applied in the field of preparing fluorine-containing secondary amines and achieves the effects of simple operation, stable chemical properties and easy system.
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Embodiment 1
[0020]
[0021] Under nitrogen protection, sequentially add [Cp*IrCl 2 ] 2 0.006mmol, 0.3mmol of aniline, 0.33mmol of fluoroethanol, 0.006mmol of sodium bicarbonate and 0.5mL of toluene, heated to 100°C and reacted for 24h. After the reaction, cool down to room temperature, add a small amount of water, extract three times with 15mL ethyl acetate, combine the organic phases, then wash with saturated brine, dry over anhydrous magnesium sulfate, evaporate the solvent under reduced pressure, and separate the secondary amine by column chromatography. 76%
Embodiment 2
[0023]
[0024] Under nitrogen protection, sequentially add [Cp*IrCl 2 ] 2 0.006 mmol, 0.3 mmol of aniline, 0.33 mmol of fluoroethanol, 0.03 mmol of triethylamine and 0.5 mL of toluene, heated to 100°C and reacted for 24 hours. After the reaction, cool down to room temperature, add a small amount of water, extract three times with 15 mL of ethyl acetate, combine the organic phases, then wash with saturated brine, dry over anhydrous magnesium sulfate, evaporate the solvent under reduced pressure, and separate the secondary amine by column chromatography. 75%.
Embodiment 3
[0026]
[0027] Under nitrogen protection, sequentially add [Cp*IrCl 2 ] 2 0.006mmol, aniline 0.3 mmol, fluoroethanol 0.33mmol, sodium bicarbonate 0.006mmol and dioxane 0.5mL, heated to 100°C and reacted for 24h. After the reaction, cool down to room temperature, add a small amount of water, extract three times with 15mL ethyl acetate, combine the organic phases, then wash with saturated brine, dry over anhydrous magnesium sulfate, evaporate the solvent under reduced pressure, and separate the secondary amine by column chromatography. 75%.
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