Novel carboxylic acid functional rhenium iron liquid and preparation method and application thereof
An ionic liquid and functional technology, applied in chemical instruments and methods, refining with oxygen-containing compounds, organic chemistry, etc., can solve problems such as poor effect and catalyst deactivation, and achieve the effect of mild conditions and simple process
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Embodiment 1
[0024] Example 1: 1-(α-carboxylic acid)methyl-3-methylimidazolium perrhenate ionic liquid
[0025] (1) Preparation of carboxylic acid functionalized rhenium ionic liquid
[0026] (1) Dissolve 0.1 mol of N-methylimidazole in absolute ethanol, add 0.1 mol of ethyl chloroacetate, reflux at 70°C for 24 hours, wash with ether, evaporate the solvent with a rotary evaporator, and dry in vacuo to obtain ions liquid intermediate A;
[0027] (2) Dissolve 0.05mol of ionic liquid intermediate A in (1), 5mL of 37% concentrated hydrochloric acid in acetonitrile, react at 70°C for 12h, cool, filter out the product, wash with ether, and dry in vacuo to obtain Intermediate B after acidification;
[0028] (3) Weigh 0.03 mol of silver perrhenate and dissolve it in acetonitrile to make it completely dissolved, add 0.03 mol of the acidified intermediate B obtained in (2), react at room temperature for 24 hours, remove the AgCl precipitate by filtration, and filter the filtrate Evaporate acetoni...
Embodiment 2
[0035] Example 2 1-(α-carboxylic acid)methyl-3-ethylimidazolium perrhenate ionic liquid
[0036] (1) Preparation of carboxylic acid functionalized rhenium ionic liquid
[0037] (1) Dissolve 0.1 mol of N-ethylimidazole in absolute ethanol, add 0.1 mol of ethyl chloroacetate, reflux at 70°C for 24 hours, wash with ether, evaporate the solvent with a rotary evaporator, and dry in vacuo to obtain ions Liquid Intermediate A.
[0038] (2) Dissolve 0.05mol of intermediate A in (1) and 5mL of 37% concentrated hydrochloric acid in acetonitrile, react at 70°C for 12h, cool, filter out the product, wash with ether, and dry in vacuo to obtain acidified Intermediate B is 1-(α-carboxylic acid)methyl-3-ethylimidazolium chloride salt.
[0039](3) Weigh 0.03 mol of silver perrhenate and dissolve it in acetonitrile to make it completely dissolved, add 0.03 mol of intermediate B obtained in (2), react at room temperature for 24 hours, filter to remove the AgCl precipitate, and rotate the filtr...
Embodiment 3
[0046] Example 3: 1-(α-carboxylic acid)methyl-3-butylimidazolium perrhenate ionic liquid
[0047] (1) Preparation of carboxylic acid functionalized rhenium ionic liquid
[0048] (1) Dissolve 0.1 mol of N-butylimidazole in absolute ethanol, add 0.1 mol of ethyl chloroacetate, reflux at 70°C for 24 hours, wash with ether, evaporate the solvent with a rotary evaporator, and dry in vacuo to obtain ions Liquid Intermediate A.
[0049] (2) Dissolve 0.05mol of intermediate A in (1) and 5mL of 37% concentrated hydrochloric acid in acetonitrile, react at 70°C for 12h, cool, filter out the product, wash with ether, and dry in vacuo to obtain acidified Intermediate B is 1-(α-carboxylic acid)methyl-3-butylimidazolium chloride.
[0050] (3) Weigh 0.03 mol of silver perrhenate and dissolve it in acetonitrile to make it completely dissolved, add 0.03 mol of intermediate B obtained in (2), react at room temperature for 24 hours, filter to remove the AgCl precipitate, and rotate the filtrate...
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