反应详情

Acid 4D (289.74 mg, 1 mmol) was dissolved in 10 ml of THF and at rt DEPC (1.1 equiv, 0.15 ml) and [2,6-bis[4-(trifluoromethyl)phenyl]-4-pyridyl]methanamine 29A (1.1 equiv., 400 mg) 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 (3:7 EtOAc:petroleum ether) afforded 140 mg of a white solid. Yield=21% 1HNMR (DMSO, 400 MHz) δ 1.25 (3H, t), 3.40 (2H, q), 4.60 (2H, d), 5.18 (1H, s), 6.18 (1H, s), 7.70 (2H, d), 7.82 (2H, d), 7.86 (4H, d), 8.02 (2H, s), 8.40 (4H, d), 8.89 (1H, bt) [M+1] 668.9 (C31H24ClF6N3O3S requires 668.05).

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 (3:7 EtOAc:petroleum ether)