反应详情

Salicylic acid (5-20 mmol) and tetrabutylphosphonium hydroxide (˜40% sol. in H2O) (3.414 g, 5 mmol) were dissolved in 20 ml of acetone stirred for 15 min at room temperature. The solvent was evaporated and the remaining viscous liquid was dried under reduced pressure (0.01 mbar, 50° C.) with stirring for 24 hrs. 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=7.74 (dd, J1=7.7 Hz, J2=1.9 Hz, 1H), 7.32 (dt, J1=7.6 Hz, J2=1.8 Hz, 1H), 6.8 (m, 2H), 2.20 (m, 4 H), 1.41 (m, 8 H), 0.9 (t, J=7.1 Hz, 6 H). 31P-NMR (121.5 MHz, d6-DMSO) δ(ppm)=35.1. 13C-NMR (75 MHz, d6-DMSO) δ(ppm)=171.9(s), 163.1(s), 131.1 (d), 129.8(d), 120.6 (s), 115.7 (d), 115.6 (d), 23.3 (d, J=16.4 Hz), 22.6 (d, J=4.8 Hz), 17.3 (d, J=47.3 Hz), 13.2 (s).

1. customThe solvent was evaporated
2. customthe remaining viscous liquid was dried under reduced pressure (0.01 mbar, 50° C.)
3. stirringwith stirring for 24 hrs