HRID720837

反应详情

EQUATION

反应方程式

HRID 720837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred mixture of 4-(3-bromophenyl)butan-1-ol (18 g) and 1,6 dibromohexane (48 ml) in 50% aq. sodium hydroxide (500 ml) with tetrabutylammonium bromide (1.5 g) was stirred for 2 d at 20°. The mixture was poured into water (1000 ml) and extracted into ethyl acetate (3×500 ml). The combined extracts were washed with water (1000 ml), dried (Na2SO4). The solvent was removed in-vacuo and the residual oil was purified by flash chromatography (500 g) using dichloromethane as eluent, changing to light petroleum (40–60°)-diethyl ether (9:1) to give the title compound (18 g). LCMS RT=4.34 min.

WORKUP

后处理

  1. extractionextracted into ethyl acetate (3×500 ml)
  2. washThe combined extracts were washed with water (1000 ml)
  3. dry with materialdried (Na2SO4)
  4. customThe solvent was removed in-vacuo
  5. customthe residual oil was purified by flash chromatography (500 g)