小中大A. 1-Butyl-3-methylimidazolium chloride . A 2-L, three-necked, round-bottomed flask is equipped with a heating oil bath, a nitrogen inlet adapter, an internal thermometer adapter, an overhead mechanical stirrer, and a reflux condenser. The flask is flushed with nitrogen and charged with 151.5 g (1.85 mol, 1 equiv) of freshly distilled N-methylimidazole (Note 1), 100 mL of acetonitrile (CH3CN, Note 2) and 220 g (2.4 mol, 1.3 equiv) of 1-chlorobutane (Note 3), and brought to a gentle reflux (75-80°C internal temperature). The solution is heated under reflux for 48 hr (Note 4) and then cooled to room temperature (Note 5). The volatile material is removed from the resulting yellow solution under reduced pressure (Note 6). The remaining light-yellow oil is re-dissolved in dry acetonitrile (250 mL) and added dropwise via cannula to a well-stirred solution of 1000 mL of dry ethyl acetate (Note 7) and one seed crystal of 1-butyl-3-methylimidazolium chloride (Note 8) placed in a 2-L, three-necked, round-bottomed flask, equipped with a nitrogen inlet adapter and an overhead mechanical stirrer (Note 9). The imidazolium salt begins to crystallize exothermically almost immediately, and after the addition of the acetonitrile solution is completed, the flask is cooled at −30°C for 2 hr. The supernatant solution is removed via filtration through a filter cannula and the resulting white solid (Note 10) is dried under reduced pressure (0.1 mbar, 0.001 mm) at 30°C for 6 hr to afford 1-butyl-3-methylimidazolium chloride 289.5 g (89%), mp 66-67°C (Notes 11 and 12).
我觉得65度是熔点吧
