反应详情

Camphorsulphonic acid (5 mmol), salicylic acid (0.6909 g, 5 mmol) and tetrabutylphosphonium hydroxide (˜40% sol. in H2O) (3.414 g, 5 mmol) were dissolved in 20 ml of acetone and stirred for 15 min at room temperature. The solvent was evaporated and the remaining viscous liquid was dried at 0.01 mbar with stirring for 24 hrs. The desired compound is isolated as a colourless liquid; 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=7.79 (dd, J1=7.9 Hz, J2=1.8 Hz), 7.52 (m, 1H), 6.94 (m, 3H), 2.97 (d, J=14.8 Hz, 1H), 2.71 (quin, J=10.8 Hz, 1H), 2.36 (d, J=14.8 Hz, 1H), 2.19 (m, 9H), 1.93 (t, J=4.5 Hz, 1H), 1.84 (m, 2H), 1.42 (m, 16 H), 1.26 (m, 2H), 1.05 (s, 3H), 0.91 (t, J=6.9 Hz, 12H), 0.74 (s, 3H). Tg−33° C., T5% onset 203° C.

1. customThe solvent was evaporated
2. customthe remaining viscous liquid was dried at 0.01 mbar
3. stirringwith stirring for 24 hrs