反应详情

To 16F (0.6 g, 1.790 mmol) in CH2Cl2 (15 mL) was added triethylamine (0.299 mL, 2.148 mmol) and MsCl (0.167 mL, 2.148 mmol). The reaction was stirred at rt for 2 h. The solvent was removed and residue was redissolved in EtOAc. The solution was washed with water and brine, dried over sodium sulfate and concentrated. The crude product was purified by flash chromatography (0-40% ETOAc/hexanes) to give 24A (0.74 g, 1.790 mmol, 100% yield) as an oil. 1H NMR (400 MHz, chloroform-d) δ ppm 7.28-7.40 (m, 7H) 7.13 (d, J=8.34 Hz, 1H) 4.39-4.59 (m, 4H) 3.69 (d, J=5.81 Hz, 2H) 3.52-3.62 (m, 1H) 2.85 (s, 3H) 2.33 (s, 3H).

1. customThe solvent was removed
2. dissolutionresidue was redissolved in EtOAc
3. washThe solution was washed with water and brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customThe crude product was purified by flash chromatography (0-40% ETOAc/hexanes)