Proline ionic liquid and preparation method and application thereof
An ionic liquid, proline technology, applied in the preparation of carboxylic acid nitrile, organic chemistry methods, chemical instruments and methods, etc., can solve the problems of difficult removal, cumbersome operation process, etc., and achieves simple separation and simple preparation process. , the effect of fast response
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Embodiment 1
[0030] (1) with N-methylimidazole and chloro-n-butane molar ratio 1: 1.1 through quaternization reaction, the reaction temperature of quaternization reaction is 70 ℃, and the reaction times is 48 hours, obtains 1-butyl- The chloride salt of 3-methylimidazole, the yield is 93.7%;
[0031] (2) neutralize proline and sodium hydroxide at room temperature in a molar ratio of 1:1 for 2 hours to obtain proline sodium salt; dissolve proline sodium salt in methanol to obtain sodium proline methanol solution;
[0032] (3) the molar ratio of the methanol solution of sodium proline obtained in step (2) and the chloride salt of 1-butyl-3-methylimidazole obtained in step (1) is 1: 0.9 and anion exchange occurs at room temperature, and the time After 12 hours, it was filtered, the solvent was removed, and the proline ionic liquid [Bmim][Pro] was obtained after drying in vacuo in a yield of 91.1%. The structure of proline ionic liquid [Bmim][Pro] is as follows:
[0033]
Embodiment 2
[0035] (1) with pyridine and bromoethane molar ratio 1: 1.4 through quaternization reaction, the reaction temperature of quaternization reaction is 100 ℃, and the reaction times is 24 hours, obtains 1-ethyl pyridinium bromide, and productive rate is 89.7 %;
[0036] (2) neutralizing L-proline and sodium hydroxide in a molar ratio of 1:1 at room temperature for 0.5 hours to obtain proline sodium salt; dissolving proline sodium salt in methanol to obtain proline sodium in methanol;
[0037] (3) with the methanol solution of step (2) gained sodium proline and step (1) gained 1-ethyl pyridine bromide in a molar ratio of 1: 0.7 at room temperature anion exchange occurs, the time is 18 hours, filtered, The solvent was removed, and the proline ionic liquid was obtained after vacuum drying, and the yield was 88.1%.
Embodiment 3
[0039] (1) with pyrrole and bromohexane molar ratio 1: 1.3 through quaternization reaction, the reaction temperature of quaternization reaction is 60 ℃, and the reaction times is 72 hours, obtains 1-ethyl pyrrole bromide, and productive rate is 91.2 %;
[0040] (2) neutralizing L-proline and sodium hydroxide in a molar ratio of 1:1 at room temperature for 3 hours to obtain proline sodium salt; dissolving proline sodium salt in methanol to obtain proline sodium in methanol;
[0041] (3) the methanol solution of sodium proline obtained in step (2) and the 1-ethylpyrrole bromide obtained in step (1) were 1:0.8 in molar ratio and anion exchange occurred at room temperature, the time was 24 hours, filtered, The solvent was removed, and the proline ionic liquid was obtained after vacuum drying, and the yield was 90.4%.
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