A high performance liquid chromatography(HPLC) method was proposed to monitor the synthesis and purification of the 1-alkyl-3-methylimidazolium ionic liquid precursors from alkylation of 1-methylimidazole with alkyl h...A high performance liquid chromatography(HPLC) method was proposed to monitor the synthesis and purification of the 1-alkyl-3-methylimidazolium ionic liquid precursors from alkylation of 1-methylimidazole with alkyl halides and determine the purity of final products.The results showed that separation of 1-methylimidazole from the precursors could be obtained under the HPLC performance conditions such as cation exchange column,acetonitrile/KH2PO4 aqueous solution and 209 nm wavelength.The content of unreacted 1-methylimidazole in the precursors could be easily calculated from their corresponding HPLC peak areas with the calibration curve of 1-methylimidazole.The retention times of the 1-alkyl-3-methylimidazolium ionic liquid precursors decreased with their increasing alkyls,and the ionic liquids with the same cation and different anions had almost the same retention times.展开更多
^1H and ^13C NMR chemical shifts were determined to investigate the interactions of acetone with a room temperature ionic liquid 1-hexyl-3- methylimidazolium bromide [C6mim]Br at various mole fractions. Changes in che...^1H and ^13C NMR chemical shifts were determined to investigate the interactions of acetone with a room temperature ionic liquid 1-hexyl-3- methylimidazolium bromide [C6mim]Br at various mole fractions. Changes in chemical shifts of hydrogen nuclei and of carbon nuclei with the acetone concentration indicated the formation of hydrogen bond between anion of the ionic liquid and methyl protons of acetone. The NMR results were in good agreement with the ab initio computational results.展开更多
文摘A high performance liquid chromatography(HPLC) method was proposed to monitor the synthesis and purification of the 1-alkyl-3-methylimidazolium ionic liquid precursors from alkylation of 1-methylimidazole with alkyl halides and determine the purity of final products.The results showed that separation of 1-methylimidazole from the precursors could be obtained under the HPLC performance conditions such as cation exchange column,acetonitrile/KH2PO4 aqueous solution and 209 nm wavelength.The content of unreacted 1-methylimidazole in the precursors could be easily calculated from their corresponding HPLC peak areas with the calibration curve of 1-methylimidazole.The retention times of the 1-alkyl-3-methylimidazolium ionic liquid precursors decreased with their increasing alkyls,and the ionic liquids with the same cation and different anions had almost the same retention times.
基金Ⅴ. ACKN0WLEDGMENTS This work was supported Science Foundation of China by the National Natural （No.20273019）.
文摘^1H and ^13C NMR chemical shifts were determined to investigate the interactions of acetone with a room temperature ionic liquid 1-hexyl-3- methylimidazolium bromide [C6mim]Br at various mole fractions. Changes in chemical shifts of hydrogen nuclei and of carbon nuclei with the acetone concentration indicated the formation of hydrogen bond between anion of the ionic liquid and methyl protons of acetone. The NMR results were in good agreement with the ab initio computational results.
