A new method for synthesizing carbamate oxime ester derivatives
A technology for the synthesis of oxime carbamate and carbamic acid, which is applied in the field of pesticide chemical synthesis, can solve the problems of poor step economy and poor compatibility of several functional groups, and achieve the effects of strong compatibility, environmental friendliness and wide substrate applicability
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Embodiment 1
[0046]Add 0.2 mmol of acetophenone oxime, 0.2 mmol of tert-butaneisonitrile, 1 mmol of water, 0.006 mmol of tris(dibenzylideneacetone) dipalladium and 0.4 mmol of acetic acid to a 25 mL test tube Sodium, add 2 ml of toluene as a solvent, stir and react at 80°C for 12 hours, stop heating and stirring, cool to room temperature, add ethyl acetate to extract three times after filtration, dry over magnesium sulfate, and remove the solvent by rotary evaporation under reduced pressure. Then separated and purified by column chromatography to obtain the target product, the column chromatography eluent used was petroleum ether:ethyl acetate mixed solvent with a volume ratio of 20:1, and the yield was 21%. The H NMR spectrum of the resulting product is shown in figure 1 As shown, the carbon NMR spectrum is shown as figure 2 , indicating that the product was successfully synthesized.
Embodiment 2
[0048] Add 0.2 mmol of l acetophenone oxime, 0.2 mmol of tert-butane isonitrile, 1 mmol of water, 0.006 mmol of bistriphenylphosphine palladium dichloride and 0.4 mmol of acetic acid in a 25 ml test tube Sodium, add 2 ml of toluene as a solvent, stir and react at 80°C for 12 hours, stop heating and stirring, cool to room temperature, add ethyl acetate to extract three times after filtration, dry over magnesium sulfate, and remove the solvent by rotary evaporation under reduced pressure. Then separated and purified by column chromatography to obtain the target product, the column chromatography eluent used was a mixed solvent of petroleum ether:ethyl acetate with a volume ratio of 20:1, and the yield was 33%. The H NMR spectrum of the resulting product is shown in figure 1 As shown, the carbon NMR spectrum is shown as figure 2 , indicating that the product was successfully synthesized.
Embodiment 3
[0050] Add 0.2 mmol of acetophenone oxime, 0.2 mmol of tert-butane isonitrile, 1 mmol of water, 0.006 mmol of tetrakistriphenylphosphopalladium and 0.4 mmol of sodium acetate in a 25 mL test tube, add 2 mL Toluene was used as a solvent. After stirring and reacting at 80°C for 12 hours, stop heating and stirring, cool to room temperature, add ethyl acetate to extract three times after filtration, dry over magnesium sulfate, remove the solvent by rotary evaporation under reduced pressure, and then pass column chromatography After separation and purification, the target product was obtained. The column chromatography eluent used was petroleum ether:ethyl acetate mixed solvent with a volume ratio of 20:1, and the yield was 68%. The H NMR spectrum of the resulting product is shown in figure 1 As shown, the carbon NMR spectrum is shown as figure 2 , indicating that the product was successfully synthesized.
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