HRID1649788

反应详情

EQUATION

反应方程式

HRID 1649788 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of propargyl alcohol (5.6 g), 1,6-dibromohexane (73.2 g), tetrabutylammonium bisulphate (0.5 g), and aqueous sodium hydroxide (50%, w/v, 27 ml) was stirred at room temperature for 20 h, diluted with water (50 ml), and extracted with diethyl ether (2×100 ml). The dried extract was evaporated and the residue was purified on a column of silica (Merck 9385) eluting with cyclohexane followed by cyclohexane-diethyl ether (19:1) to give the title compound as a colourless oil (15.0 g), t.l.c. (cyclohexane-diethyl ether 9:1) Rf 0.4.

WORKUP

后处理

  1. extractionextracted with diethyl ether (2×100 ml)
  2. extractionThe dried extract
  3. customwas evaporated
  4. customthe residue was purified on a column of silica (Merck 9385)
  5. washeluting with cyclohexane