反应详情

温度

0 °C

A solution of the product from Step B (0.130 g; 0.282 mmol) in THF (3 mL) cooled to 0° C. was treated with 1 M solution of lithium bis(trimethylsilyl)amide in THF (0.85 mL; 0.85 mmol) and stirred at 0° C. under nitrogen for 30 minutes. The reaction mixture was quenched at 0° C. with 10% aqueous NaHSO4 solution. The reaction mixture was partitioned between ethyl acetate and 10% NaHSO4 aqueous solution. The organic layer was washed twice with saturated NaHCO3 solution, brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by MPLC (silica gel; 0% to 20% ethyl acetate:hexane gradient) gave the title compound. HPLC/MS: 460.9 (M+1), 462.9 (M+3); Rt=4.35 min.

1. customThe reaction mixture was quenched at 0° C. with 10% aqueous NaHSO4 solution
2. customThe reaction mixture was partitioned between ethyl acetate and 10% NaHSO4 aqueous solution
3. washThe organic layer was washed twice with saturated NaHCO3 solution, brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification by MPLC (silica gel; 0% to 20% ethyl acetate:hexane gradient)