反应详情

温度

0 °C

To a suspension of the hydroxy ester of Step 3 (4.519 g, 9.5 mmol) and N,O-dimethylhydroxylamine hydrochloride (2.777 g, 28.5 mmol) in 95 mL of anhydrous THF at 0° C. was added dropwise 3M EtMgBr in Et2O (22 mL 66 mmol) over ≃40 min. The mixture was then stirred at 0° C. for 30 min. and poured into ice-cold saturated NH4Cl. The product was extracted in EtOAc, dried over Na2SO4, and concentrated to yield the title compound.

1. additionpoured into ice-cold saturated NH4Cl
2. extractionThe product was extracted in EtOAc
3. dry with materialdried over Na2SO4
4. concentrationconcentrated