HRID882926

反应详情

EQUATION

反应方程式

HRID 882926 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 (R)-4-(4-{3-[4-(3-bromo-propyl)-phenoxy]-propyl}-phenoxymethyl)-2,2-dimethyl-[1,3]dioxolane (5.0 g, 10.8 mmol) in DCM (50 mL) is added TFA (2.0 mL, 26.9 mmol) dropwise followed by water (2.0 mL) and the reaction mixture is stirred at RT overnight. The solvent is removed in vacuo and the residue is treated with aqueous sodium hydrogen carbonate solution. The mixture is extracted with EtOAc (3×200 mL) and the combined organic portions are washed with water, brine, dried over Na2SO4 and concentrated in vacuo. Recrystallizisation of the residue from diethyl ether-hexane affords the title compound as white solid.

WORKUP

后处理

  1. customThe solvent is removed in vacuo
  2. additionthe residue is treated with aqueous sodium hydrogen carbonate solution
  3. extractionThe mixture is extracted with EtOAc (3×200 mL)
  4. washthe combined organic portions are washed with water, brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo