HRID500531

反应详情

EQUATION

反应方程式

HRID 500531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The crude product of the title compound from Example 13.1 (50.0 mg, 0.158 mmol) was weighed into a vial and toluene (3 mL) was added. Potassium carbonate (47.0 mg, 0.340 mmol) and lead (IV) acetate (70.0 mg, 0.158 mmol) were added with stirring. The reaction was allowed to stir for 2.5 hours. The reaction was filtered and ethyl acetate was added to the filtrate and an aqueous workup was done. The organic layer was washed with brine, dried over sodium sulfate, filtered and concentrated. The crude product was purified by column chromatography (40% EtOAc/hexanes) to yield the pure product as a white solid (22.3 mg, 68%).

WORKUP

后处理

  1. additionwas added
  2. stirringto stir for 2.5 hours
  3. filtrationThe reaction was filtered
  4. additionethyl acetate was added to the filtrate
  5. washThe organic layer was washed with brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude product was purified by column chromatography (40% EtOAc/hexanes)