HRID1463365

反应详情

EQUATION

反应方程式

HRID 1463365 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 benzenesulphinic acid (8.68 g, 0.061 M) in DCM (120 ml) containing a suspension of CaCl2 (1.0 g) at room temperature was added a solution of 2-(3,4,dimethoxybenzyl)-5-methoxytetrahydrofuran (7.0 g, 0.029 M) in CH2Cl2 (80 ml). The mixture was stirred at room temperature for 4 h, quenched by washing with water (2×50 ml), dried (Na2SO4) and evaporated. Column chromatography (flash silica gel, hexane:ethyl acetate (3:2)) provided the product (Rf 0.3) as a clear oil which was crystallised from ethyl acetate/hexane to give 2-benzenesulphonyl-5-(3,4-dimethoxyphenyl)tetrahydrofuran (3.5 g, 35%).

WORKUP

后处理

  1. customquenched
  2. washby washing with water (2×50 ml)
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customColumn chromatography (flash silica gel, hexane:ethyl acetate (3:2)) provided the product (Rf 0.3) as a clear oil which
  6. customwas crystallised from ethyl acetate/hexane