1-BUTYL-3-METHYLIMIDAZOLIUM BIS(TRIFLUOR

4316-42-1

77-78-1

174899-83-3

The general procedure for the synthesis of 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide from N-butylimidazole and dimethyl sulfate is as follows: 1. 620.5 g (5 mol) of N-butylimidazole was added to a 5 liter reaction vessel, followed by the addition of 630.5 g (5 mol) of dimethyl sulfate in batches. 2. the mixture was stirred for 15 minutes to ensure adequate reaction. 3. 1435.3 g (5 mol) of lithium bis(trifluoromethanesulfonyl)imide dissolved in 2 liters of water was added to the reaction mixture, and the formation of a second liquid phase of the product was immediately observed. 4. Phase separation was carried out and the organic phase was collected and dried under high vacuum (HV) at 60 °C to afford 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide in 98% yield. 5. To detect residual chlorides, about 1 g of the product was dissolved in 5 ml of water, acidified with 2 drops of concentrated nitric acid and then 3-4 drops of silver nitrate solution were added. No precipitation of silver chloride was observed indicating that no halide ions remained in the product. 6. 6. The 1H-NMR (300 MHz, acetone-d3) data of the product were as follows: 0.95 (3H, t, J=9.2 Hz, Hh); 1.33-1.39 (2H, m, Hg); 1.90-2.00 (2H, m, Hf); 4.07 (3H, s, Hb); 4.37 (2H, t, J=9.3 Hz, He); 7.71 (1H, t, J=9.3 Hz, Hb); 7.76 (1H, s, Hb); 4.37 (2H, t, J=9.3 Hz, He); and 7.71 (1H, s, Hb). ,7.76 (1H, s, Hc, d); 9.02 (1H, s, Ha) ppm.