Annular guanidinium ionic liquid and preparation method therof
A technology of ionic liquid and cyclic guanidine, which is applied in the field of cyclic guanidine salt ionic liquid and its preparation, achieves mild reaction conditions, is conducive to large-scale industrial production, and is easy to realize
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Embodiment 11
[0037] Embodiment 11, the synthesis of 3-dimethyl-2-pyrrolidinyl-imidazolium iodide ionic liquid
[0038] 1) Dissolve 0.3 mol of 1,3-dimethyl-2-imidazolidinone in 50 ml of toluene, then slowly add 0.3 mol of phosphorus oxychloride dropwise, react at 65°C for 12 hours, and generate "Vilsmeier salt";
[0039] 2) After the formation of "Vilsmeier salt", add 50ml of dichloromethane, slowly add 0.6mol of pyrrolidine dropwise, reflux at 65°C for 12 hours, and drop in 35% NaOH aqueous solution after cooling to make the system alkaline (PH7.5) , and then the reaction mixture was extracted 3 times with dichloromethane, and the extracted organic phases were combined and washed with anhydrous MgSO 4 After drying to remove moisture, the organic phase was distilled off under reduced pressure to obtain a cyclic guanidine salt.
[0040] The synthetic chemical expression of described cyclic guanidine salt is as follows:
[0041]
[0042] 3) Dissolve 0.3 mol of cyclic guanidine salt in 100 ...
Embodiment 2
[0043] Embodiment 2: Synthesis of 1,3-dimethyl-2-pyrrolidinyl-imidazolium iodide ionic liquid
[0044] 1) Dissolve 0.3 mol of 1,3-dimethyl-2-imidazolidinone in 50 ml of toluene, then slowly add 0.3 mol of phosphorus oxychloride dropwise, react at 60°C for 10 hours, and generate "Vilsmeier salt";
[0045] 2) After the "Vilsmeier salt" is generated, add 50ml of dichloromethane, slowly add 0.6mol of pyrrolidine dropwise, reflux at 60°C for 20 hours, and drop in 35% NaOH aqueous solution after cooling to make the system alkaline (PH9), Then the reaction mixture was extracted 3 times with dichloromethane, and the extracted organic phases were combined and washed with anhydrous MgSO 4 After drying to remove moisture, the organic phase was distilled off under reduced pressure to obtain a cyclic guanidine salt.
[0046] 3) Dissolve 0.3 mol of cyclic guanidine salt in 100 ml of acetone, add 0.3 mol of methyl iodide aqueous solution containing methyl iodide under nitrogen protection, a...
Embodiment 3
[0047] Example 3: Synthesis of hexafluorophosphate-1,3-dimethyl-2-pyrrolidinyl-imidazolium salt ionic liquid
[0048] Dissolve 0.3 mol of 1,3-dimethyl-2-pyrrolidinyl-imidazolium iodide ionic liquid in 100 ml of acetone, and add 0.3 mol of KPF under nitrogen protection 6 The aqueous solution was reacted at 65°C for 10 hours, and the solvent acetone was removed under reduced pressure to obtain the target product hexafluorophosphate-1,3-dimethyl-2-pyrrolidinyl-imidazole ionic liquid.
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