反应详情

温度

0 °C

Intermediate D4 (1.1 g, 2.80 mmol) was dissolved in THF (15 ml) and iron(III) acetylacetonate (0.099 g, 0.28 mmol) and NMP (1 ml) were added. The reaction mixture was then cooled to 0° C. Under N2 (gas) protection, CH3MgBr 3M in Et2O (4 ml, 12 mmol) was added slowly. The reaction mixture was warmed to room temperature and stirred for one hour until the reaction was finished. The reaction mixture was then quenched with saturated NH4Cl solution and then extracted by CH2Cl2 (3×30 ml). The combined organic phase was washed by brine, dried over MgSO4, filtered and the solvent was evaporated in vacuo. The residue was purified by reversed-phase high-performance liquid chromatography (Shandon Hyperprep® C18 BDS (Base Deactivated Silica) 8 μm, 250 g, I.D. 5 cm). A gradient with 2 or 3 mobile phases was applied (phase A: a 0.25% NH4HCO3 solution in water; phase B: CH3OH (optional); phase C: CH3CN).

1. temperatureThe reaction mixture was warmed to room temperature
2. customThe reaction mixture was then quenched with saturated NH4Cl solution
3. extractionextracted by CH2Cl2 (3×30 ml)
4. washThe combined organic phase was washed by brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customthe solvent was evaporated in vacuo
8. customThe residue was purified by reversed-phase high-performance liquid chromatography (Shandon Hyperprep® C18 BDS (Base Deactivated Silica) 8 μm, 250 g, I.D. 5 cm)