HRID11741

反应详情

EQUATION

反应方程式

HRID 11741 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-50 °C

PROCEDURE

实验过程

To a solution of fluorene (33.2 g, 0.20 mol) in 300 mL THF at −78° C., n-butyllithium (2.5 M, 80 mL) was added dropwisely. The mixture was stirred at −50° C. for 45 minutes, and then cooled to −78° C. again and n-hexylbromide (33.0 g, 0.20 mol) in THF (25 mL) was added dropwise to the mixture. The solution was allowed to warm up to room temperature and stirred for 5 h. The mixture was then poured into water and extracted with ether. The organic extracts were washed with brine and dried over magnesium sulfate, and purified by silica gel column with hexane to give pure compound 2 (38 g, yield 76%).

WORKUP

后处理

  1. temperaturecooled to −78° C. again
  2. temperatureto warm up to room temperature
  3. stirringstirred for 5 h
  4. extractionextracted with ether
  5. washThe organic extracts were washed with brine
  6. dry with materialdried over magnesium sulfate
  7. custompurified by silica gel column with hexane