HRID567950

反应详情

EQUATION

反应方程式

HRID 567950 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 4-{2-[3,4-bis(difluoromethoxy)phenyl]-2-{6-[4-(methoxycarbonyl)phenoxy]-3-pyridyl}ethyl}pyridine from Example 1 (249 mg, 0.46 mmol) in a mixture of 5 mL of CH2Cl2 and 0.5 mL of MeOH, was added MMPP (171 mg, 0.28 mmol) in one portion. The mixture was stirred 24 h at room temperature, quenched with a saturated aqueous NaHCO3 solution and diluted with CH2Cl2. The organic layer was washed with brine, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (Gradient 20% to 40% EtOHiethyl acetate) to afford the title compound as a viscous oil (260 mg, 71%).

WORKUP

后处理

  1. customquenched with a saturated aqueous NaHCO3 solution
  2. additiondiluted with CH2Cl2
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by flash chromatography on silica gel (Gradient 20% to 40% EtOHiethyl acetate)