HRID1033875

反应详情

EQUATION

反应方程式

HRID 1033875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 100 mL Schlenk flask is charged with diethyl ether, 50 mL, and n-butyllithium, 5.5 mL of a 2.78M solution is hexane (16 mmoles), while stirring magnetically and maintaining the temperature at or below -20° C. in a dry ice/acetone bath. Nitrogen degassed indene, 2.0 mL (16.8 mmole), is added to the chilled, stirred solution. The mixture is warmed to room temperature and stirred approximately 15 hours followed by refluxing for 1 hour. The reaction is assumed to be stoichiometric and complete based on titration data obtained from previous preparations of lithium indenide.

WORKUP

后处理

  1. temperaturemaintaining the temperature at or below -20° C. in a dry ice/acetone bath
  2. customNitrogen degassed indene, 2.0 mL (16.8 mmole)
  3. additionis added to the chilled
  4. stirringstirred solution
  5. stirringstirred approximately 15 hours
  6. temperatureby refluxing for 1 hour