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2 is as follows. 2 ml (or 2 g) of amine, 3 ml of ionic liquid and 0.05 g of base were put into an autoclave (100 ml) with a magnetic stirring bar. Carbon dioxide (60 atm, purity > 99 %) was introduced into the reactor, and the reaction was stirred and heated at 170°C for 4-36 h. Water (10 mL) was added into the resulting reaction mixture, and the desired resulted product precipitated out. The solid product was recovered by filtration, washing and drying. Ionic liquid containing CsOH could also be recovered and reused after the filtrate was distillated to remove water. All products were qualitatively analyzed with a HP 6890/5973 GC-MS and quantitatively analyzed with HP 1790GC (flame ion detector).
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note
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When using CsOH/CMImCl, a foamy mixture resulted that could not be separated effectively, although the conversion of cyclohexylamine was analyzed by GC and found to be > 95 %.
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note
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The by-products formed in the reactions were only carbamic salts, which readily dissolved in water.
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