反应详情

温度

120 °C

The product of step A (200 mg, 0.42 mmol) was dissolved in toluene (2 mL) and p-toluenesulfonic acid (30 mg, 0.16 mmol) was added. The reaction was heated at 120° C. for 4 h and allowed to cool overnight. The reaction was diluted with EtOAc and washed with a saturated solution of NaHCO3, brine, dried (Na2SO4), filtered and concentrated The residue was purified by flash chromatography on silica gel gradient eluted with 0-30% EtOAc in hexane to afford the title compound. (LC-2) HPLC/MS: 464.2 (M+1), 466.2 (M+3); Rt=2.61 min.

1. temperatureto cool overnight
2. washwashed with a saturated solution of NaHCO3, brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated The residue
6. customwas purified by flash chromatography on silica gel gradient
7. washeluted with 0-30% EtOAc in hexane