Oxaallylamine compound as well as preparation method and application thereof
A technology of oxaallylamine and allylamine, which is applied in the field of oxaallylamine compounds and their preparation, can solve the problem that there are few synthesis methods of oxaallylamine compounds that do not conform to the development of green chemistry No concept, no application prospects, etc., to achieve the effect of novel and efficient synthetic methods, wide applicability of substrates, and high atom utilization
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Embodiment 2
[0066] In the sealed tube, first add 0.01 mmol of copper acetate, 0.01 mmol of zinc chloride dissolved in 1.0 ml of dichloromethane solvent, and finally add 0.2 mmol of N-methyl-1-naphthylamine and 0.3 mmol of phenyl Allene ether was stirred and reacted at 50 degrees Celsius at 700 rpm for 6 hours, and the stirring was stopped. Add 5 mL of water, extract 3 times with ethyl acetate, combine the organic phases and use 0.5 g of anhydrous sodium sulfate to dry, filter, concentrate under reduced pressure, and then separate and purify by thin-layer chromatography to obtain the target product, the thin-layer chromatography used The developer is petroleum ether:ethyl acetate mixed solvent with a volume ratio of 200:1, and the yield is 82%.
[0067] The hydrogen spectrogram and the carbon spectrogram of the product obtained in this embodiment are respectively as follows image 3 and Figure 4 shown; the structural characterization data are shown below:
[0068] 1 H NMR (400MHz, CDC...
Embodiment 3
[0075] In the sealed tube, first add 0.01 mmol of copper acetate, 0.01 mmol of zinc chloride dissolved in 1.0 ml of dichloromethane solvent, and finally add 0.2 mmol of N-allylaniline and 0.3 mmol of phenyl allenyl ether , stirred and reacted at 50 degrees Celsius at 700 rpm for 6 hours, and stopped stirring. Add 5 mL of water, extract 3 times with ethyl acetate, combine the organic phases and use 0.5 g of anhydrous sodium sulfate to dry, filter, concentrate under reduced pressure, and then separate and purify by thin-layer chromatography to obtain the target product, the thin-layer chromatography used The developer is petroleum ether:ethyl acetate mixed solvent with a volume ratio of 200:1, and the yield is 81%. The hydrogen spectrogram and the carbon spectrogram of the product obtained in this embodiment are respectively as follows Figure 5 and Figure 6 shown; the structural characterization data are shown below:
[0076] 1 H NMR (400MHz, CDCl 3 )δppm 7.32(t, J=8.0Hz,...
Embodiment 4
[0083] In the sealed tube, first add 0.01 mmol of copper acetate, 0.01 mmol of zinc chloride dissolved in 1.0 ml of dichloromethane solvent, and finally add 0.2 mmol of 2,4-dichloroaniline and 0.3 mmol of phenylalkene Ether, stirred and reacted at 50 degrees Celsius at 700 rpm for 6 hours, and stopped stirring. Add 5 mL of water, extract 3 times with ethyl acetate, combine the organic phases and use 0.5 g of anhydrous sodium sulfate to dry, filter, concentrate under reduced pressure, and then separate and purify by thin-layer chromatography to obtain the target product, the thin-layer chromatography used The developer is petroleum ether:ethyl acetate mixed solvent with a volume ratio of 500:1, and the yield is 70%.
[0084] The hydrogen spectrogram and the carbon spectrogram of the product obtained in this embodiment are respectively as follows Figure 7 and Figure 8 shown; the structural characterization data are shown below:
[0085] 1 H NMR (400MHz, CDCl 3 )δppm 7.33(...
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