Application of ethyl-sulfuric acid compound and preparation method thereof
A technology of ethyl sulfuric acid and solvate, which is applied in the application and preparation of ethyl sulfuric acid compounds, can solve the problems of undiscovered medical uses of ethyl sulfuric acid compounds, and achieve good anti-inflammatory effects
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Embodiment 1
[0056] Embodiment 1: the preparation of sodium ethyl sulfate
[0057] Add a certain amount of ethanol to the reaction kettle, slowly add 6 times the amount of sulfuric acid ethanol solution dropwise under stirring, control the temperature of the reaction kettle at 38°C, and continue stirring for 24 hours for the esterification reaction. Add ethanol, stir well, adjust the pH to 7.0 with 10% NaOH, add 95% ethanol to make the alcohol content reach more than 85%, recover ethanol under reduced pressure, and separate the aqueous solution through adsorption resin column chromatography, and use water: ethanol gradient elution, Collect the eluate fraction containing sodium ethyl sulfate compound, crystallize to obtain sodium ethyl sulfate, ESIMS m / z171[M+Na] + ,319[2M+Na] + ,125[M–Na] – , 273[2M–Na] – ; 1 H (400MHz, CD 3 OD) and 13 C NMR (100MHz, CD 3 OD),
[0058] 1 NMR (CD 3 OD, 400MHz) δ: 1.38(t, J=7.2Hz, 3H, H-1), 4.16(q, J=7.2Hz, 2H, H-2),
[0059] 13 C-NMR (CD 3 OD, ...
Embodiment 2
[0060] Embodiment 2: the preparation of sodium ethyl sulfate
[0061] Add a certain amount of ethanol to the reaction kettle, slowly add 4 times the same amount of sulfuric acid methanol solution dropwise under stirring, control the temperature of the reaction kettle at 40°C, and continue stirring for 30 hours for the esterification reaction. Add methanol, stir well, wash with 10% NaHCO 3 Adjust the pH to 5.5, add 90% methanol to make the alcohol content reach more than 85%, recover methanol under reduced pressure, and separate the aqueous solution through adsorption resin column chromatography, and use water:methanol gradient elution to collect the eluted compounds containing sodium ethyl sulfate. Liquid components, crystallization, that is, sodium ethyl sulfate.
[0062] Sodium ethyl sulfate mass spectrometry and NMR data are the same as in Example 1.
Embodiment 3
[0063] Embodiment 3: the preparation of sodium ethyl sulfate
[0064] Add a certain amount of ethanol to the reaction kettle, slowly add 6 times the equivalent amount of sulfuric acid ethanol solution dropwise under stirring, control the temperature of the reaction kettle at 40°C, and continue stirring for 36 hours for the esterification reaction. Add ethanol, stir well, and use 10% Na 2 CO 3 Adjust the pH to 6.0, add 95% ethanol to make the alcohol content reach more than 88%, recover isopropanol under reduced pressure, and separate the aqueous solution through adsorption resin column chromatography, elute with water: isopropanol alcohol gradient, and collect ethyl sulfuric acid The eluent component of the sodium compound is crystallized to obtain sodium ethyl sulfate.
[0065] Sodium ethyl sulfate mass spectrometry and NMR data are the same as in Example 1.
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