反应详情

Acid 18 (0.3 g, 1.09 mmol) was dissolved in 15 ml of THF and at rt DEPC (1.3 equiv, 0.21 mL) and [2-[4-(trifluoromethyl)phenyl]-4-pyridyl]methanamine 21A (1.1 mol equiv., 0.37 g) were added to the solution. The mixture was stirred at rt overnight then evaporated. The residue 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 by chromatographic column (EtOAc 3/petroleum ether 7) afforded 100 mg of a white solid. Yield=18% 1HNMR (DMSO, 200 MHz) δ 1.24 (m, 5H), 1.35 (m, 2H), 3.45 (m, 2H), 4.44 (d, 2H, J=6.2), 7.26 (m, 3H), 6.61 (d, 1H, J=2.1), 7.88 (d, 2H, J=7.8), 7.94 (s, 1H), 8.31 (d, 3H, J=8), 8.64 (d, 1H, J=4.1). [M+1] 543.95 (C23H21ClF3N3O3S2 requires 544.01).

1. additionwere added to the solution
2. customthen evaporated
3. dissolutionThe residue was dissolved in AcOEt (30 mL)
4. washwashed with water (1×20 mL) and brine
5. dry with materialThe organic phase was dried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customThe purification of the crude by chromatographic column (EtOAc 3/petroleum ether 7)