反应详情

温度

60 °C

To a solution of 3-Methyl-1-(propoxyethoxycarbonylmethyl)imidazolium bromide (3.32 g, 12.0 mmol) in distilled water (20 mL) was added in one portion sodium octyl sulfate (2.09 g, 9.00 mmol) and stirred at 60° C. for 2 h. The water was then slowly removed under vacuum. The precipitate was dissolved in DCM (10 mL) and washed with distilled water (2×5 mL). The product remaining was dried on the rotary evaporator and then under high vacuum for 8 h to yield a dark yellow grease at RT in 85% yield (3.33 g, 7.64 mmol). 1H δ ppm 9.45 (s, 1H), 7.48 (t, J=1.6 Hz, 1H), 7.41 (t, J=1.6 Hz, 1H), 5.25 (5, 2H), 4.36 (t, J=4.8 Hz, 2H), 4.01 (s, 3H), 3.67 (t, J=4.6 Hz, 2H), 3.43 (t, J=6.8 Hz, 2H), 1.63-1.58 (m, 2H), 0.92-0.86 (m, 3H) 13C δ ppm 166.45, 138.89, 123.71, 123.06, 73.04, 67, 92, 67.89, 65.67, 49.91, 36.58, 31.83, 29.50, 29.36, 29.26, 25.87, 22.73, 22.66, 14.13, 10.47

1. customThe water was then slowly removed under vacuum
2. dissolutionThe precipitate was dissolved in DCM (10 mL)
3. washwashed with distilled water (2×5 mL)
4. customThe product remaining was dried on the rotary evaporator
5. customunder high vacuum for 8 h to yield a dark yellow grease at RT in 85% yield (3.33 g, 7.64 mmol)