反应详情

温度

50 °C

To the product of Example 1 Step B (7.0 g, 18.6 mmol in THF (90 mL) was added MeMgBr (1.4 M in toluene/THF, 14 mL, 19.6 mmol). After stirring for 3 min, prop-1-enylmagnesium bromide (0.5 M in THF, 55.9 mL, 28 mmol) was added and the temperature was increased to 50° C. The reaction was quenched with 2 M HCl after 30 min and diluted with EtOAc. The solution was washed with brine, and concentrated The residue was purified by flash chromatography on silica gel gradient eluted with 0-35% EtOAc in hexane to afford the title compound. (LC-2) HPLC/MS: 418.2 (M+1), 420.2 (M+3); Rt=4.08 min.

1. customThe reaction was quenched with 2 M HCl after 30 min
2. additiondiluted with EtOAc
3. washThe solution was washed with brine
4. concentrationconcentrated The residue
5. customwas purified by flash chromatography on silica gel gradient
6. washeluted with 0-35% EtOAc in hexane