反应详情

To a solution of 153A (627 mg, 2 mmol) in DMF (5 mL) at RT was added NaH (96 mg, 2.4 mmol) in portions. After addition, the reaction was stirred at RT for 30 min, and then 2-(trimethylsilyl)ethoxymethyl chloride (0.37 mL, 2.10 mmol) was added dropwise. After addition, the reaction was stirred at RT for 1 h, then quenched carefully with water. The mixture was extracted with EtOAc (3×30 mL), and the combined extracts washed with brine, dried (Na2SO4), and concentrated. The resulting residue was chromatographed (silica gel) eluting with EtOAc (0-60%) in hexane to give the title compound as a white powder (620 mg, 70%).

1. additionAfter addition
2. additionAfter addition
3. stirringthe reaction was stirred at RT for 1 h
4. customquenched carefully with water
5. extractionThe mixture was extracted with EtOAc (3×30 mL)
6. washthe combined extracts washed with brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated
9. customThe resulting residue was chromatographed (silica gel)
10. washeluting with EtOAc (0-60%) in hexane