反应详情

To the product of Example 1 (59.5 mg) in THF (2 mL) at 0° C. was added 0.52 mL MeMgBr solution (1.4 M, 75% toluene/25% THF). After 10 min the reaction was quenched with saturated aqueous NH4Cl and then diluted with EtOAc. The solution was washed with 10% aqueous NaHSO4 followed by aqueous NaHCO3/NaOH (4:1) before drying (Na2SO4). The concentrated residue was purified by preparative TLC (silica gel) eluted with 15% EtOAc in hexane affording the title compound. HPLC/MS: 512.0 (M+1), 514.0 (M+3); Rt=5.14 min.

1. customAfter 10 min the reaction was quenched with saturated aqueous NH4Cl
2. additiondiluted with EtOAc
3. washThe solution was washed with 10% aqueous NaHSO4
4. dry with materialbefore drying (Na2SO4)
5. customThe concentrated residue was purified by preparative TLC (silica gel)
6. washeluted with 15% EtOAc in hexane affording the title compound