反应详情

To a solution of compound 3A (124 mg, 0.30 mmol) in THF (5 mL) at 0° C. was slowly added a 3.0 M solution of MeMgBr in ether (0.40 mL, 1.20 mmol. The reaction was warmed to room temperature and then heated at 50° C. for 1 h. After cooling to room temperature, the reaction was quenched with EtOAc (20 mL) and saturated aqueous NH4Cl (20 mL) was added. The resulting two layers were separated and the organic layer washed with brine, dried over Na2SO4 and concentrated to an orange oil. This crude oil was purified by silica gel flash chromatography (eluted with 14-17% EtOAc/CH2Cl2) to give compound 145 as a yellow solid (76 mg, 64%). HPLC: 97% at 1.97 min (retention time) (Phenom-Prime S5 C18 column, 4.6×30 mm, eluting with 10-90% aqueous methanol over 2 min containing 0.1% TFA, 5 mL/min, monitoring at 220 nm). MS (ES): m/z 399 [M+H]+.

1. temperatureheated at 50° C. for 1 h
2. temperatureAfter cooling to room temperature
3. customthe reaction was quenched with EtOAc (20 mL) and saturated aqueous NH4Cl (20 mL)
4. additionwas added
5. customThe resulting two layers were separated
6. washthe organic layer washed with brine
7. dry with materialdried over Na2SO4
8. concentrationconcentrated to an orange oil
9. customThis crude oil was purified by silica gel flash chromatography (eluted with 14-17% EtOAc/CH2Cl2)