Compound containing multielement alkamines, and preparation method and application thereof
A technology for amino alcohols and compounds, which is applied in the preparation of amino hydroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc. Weakness and other problems, to achieve the effect of dense protective film, improved corrosion resistance, and stable adsorption
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Embodiment 1
[0035] Take 18.5g epichlorohydrin and join in the reactor that 10ml water is housed, keep reaction temperature 20 ℃, add 18g dimethylamine and 0.27g AlCl while stirring 3 (The molar ratio of the three substances, 1:2:0.001), continued stirring for 4 hours, then stopped stirring, and added 10 mL of 30% NaOH solution to obtain a dibasic amino alcohol compound.
[0036] The yield of the above-mentioned derivatives having an aminoalcohol structure was determined to be 93% by liquid chromatography. After the above-mentioned derivatives with aminoalcohol structure are purified by column chromatography (using silica gel as filler, the eluent is composed of acetone and ethyl acetate mixed, wherein the volume ratio of acetone and ethyl acetate is 1:10), The structure was confirmed by proton nuclear magnetic resonance spectrum and infrared spectrum, and the results are as follows:
[0037] 1H-NMR (400MHz, CDCl3, δ, ppm) δ2.5(s, 12H), 2.3(d, J=6.4Hz, 4H), 3.5(t, 1H), 3.6(d, OH, 1H);
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Embodiment 2
[0042] Get 18.5g epichlorohydrin and join in the reactor that 10ml water is housed, after being warmed up to 60 ℃, add 44.4g di-n-propylamine and 0.54g zinc dichloride while stirring (three kinds of material molar ratio, 1: 2.2 : 0.002), keep the reaction temperature at 60°C, continue to stir and react for 4h, then stop heating. After cooling, add 10 mL of 30% NaOH solution and stir evenly to obtain a derivative with an amino alcohol structure.
[0043] The yield of the above-mentioned derivatives having an aminoalcohol structure was determined to be 91% by liquid chromatography. After the above-mentioned derivatives with aminoalcohol structure are purified by column chromatography (using silica gel as filler, the eluent is composed of acetone and ethyl acetate mixed, wherein the volume ratio of acetone and ethyl acetate is 1:15), The structure was confirmed by proton nuclear magnetic resonance spectrum and infrared spectrum, and the results are as follows:
[0044] 1H-NMR (...
Embodiment 3
[0049] Get 18.5g epichlorohydrin and join in the reactor that 10ml dehydrated alcohol is housed, after being warmed up to 50 ℃, add 36g ethylenediamine and 1.63g iron trichloride (three kinds of material mol ratios, 1: 3:0.005), keep the reaction temperature at 50°C, continue to stir and react for 8 hours, then stop heating, add 10mL 30% NaOH solution after cooling and stir evenly to obtain derivatives with aminoalcohol structure.
[0050] The yield of the above-mentioned derivatives having an aminoalcohol structure was determined to be 92% by liquid chromatography. After the above-mentioned derivatives with aminoalcohol structure are purified by column chromatography (using silica gel as filler, the eluent is composed of acetone and ethyl acetate mixed, wherein the volume ratio of acetone and ethyl acetate is 1:10), The structure was confirmed by proton nuclear magnetic resonance spectrum, infrared spectrum and gas chromatography-mass spectrometry. The results are as follows:...
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