HRID600141

反应详情

EQUATION

反应方程式

HRID 600141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

n-Butyl lithium (7.6 ml, 19.1 mmols, 2.52 M) was added to a 30 ml THF solution of 1-pentyne (2.05 ml, 21.06 mmols) at −78° C., and the mixture was stirred at room temperature for an hour. 2,3-Bis(bromomethyl)-1,4-dipropylnaphthalene (1.91 g, 4.79 mmols) and DMPU (2.3 ml, 19.1 mmols) were added to the mixture at room temperature. After stirring for an hour, the mixture was treated with 3N HCl and extracted with hexane. The extract was then washed with sodium hydrogencarbonate aqueous solution and brine, followed by drying over anhydrous magnesium sulfate. Column chromatography was performed using silica gel as the packing material to give the title compound (1.66 g) as a white solid. The isolation yield was 93%

WORKUP

后处理

  1. stirringAfter stirring for an hour
  2. extractionextracted with hexane
  3. washThe extract was then washed with sodium hydrogencarbonate aqueous solution and brine
  4. dry with materialby drying over anhydrous magnesium sulfate