HRID8823

反应详情

EQUATION

反应方程式

HRID 8823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the product of Step A in 4 mL DMF was added 0.125 g (0.698 mmol) of 1-bromopinacolone and 0.455 g (1.39 mmol) of Cs2CO3. The reaction mixture was stirred at room temperature for 1 h, then partitioned between EtOAc and saturated aqueous NaHCO3 solution. The organic layer was separated, washed with aq. NaHCO3, brine, dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–75% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound.

WORKUP

后处理

  1. custompartitioned between EtOAc and saturated aqueous NaHCO3 solution
  2. customThe organic layer was separated
  3. washwashed with aq. NaHCO3, brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified on a silica gel flash chromatography column
  8. washeluted with 0–75% EtOAc-hexane
  9. customEvaporation of the purified fractions
  10. customdrying in vacuo