反应详情

温度

80 °C

4-trifluoromethylphenylacetic acid (453 mg, 2.2 mmol) was dissolved in 20 ml of THF and at 0° C. DEPC (0.43 ml, 1.3 equiv) and amine 1c (400 mg, 2.66 mmol) were added to the solution. The mixture was warmed at 80° C. overnight, then evaporated and the crude was dissolved in AcOEt (30 ml) and washed with water (1×20 ml) and brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The purification of the crude residue by chromatographic column using AcOEt 3/petroleum ether 7 as eluant gave 340 mg of a white solid. Yield=46% 1HNMR (DMSO, 200 MHz) δ 3.86 (2H, s), 6.86 (1H, d), 7.06 (1H, t), 7.58 (3H, m), 7.70 (2H, d, J=8.4 Hz), 10.32 (1H, bs), 8.73 (1H, bs), 11.80 (1H, bs); [M+1] 337.2 (C16H11F3N2O3 requires 336.3).

1. customevaporated
2. dissolutionthe crude was dissolved in AcOEt (30 ml)
3. washwashed with water (1×20 ml) and brine
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated under vacuum
6. customThe purification of the crude residue by chromatographic column