HRID369480

反应详情

EQUATION

反应方程式

HRID 369480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Into a two-necked round-bottomed flask, the atmosphere in which was replaced with nitrogen, were charged 30 g of tetrahydrofuran and 1.10 g of tetramethylcyclopentadiene. The mixture was cooled to 0° C. with stirring and 4.90 ml of n-butyl lithium (1.6M solution in n-hexane) (7.84 mmol as n-butyl lithium) was gradually added dropwise thereto over 20 minutes. The obtained reaction mixture in the form of a white slurry was stirred further for at 0° C. for 3 hours, and added to a pre-cooled mixed solution of tetrahydrofuran (10 g) and n-hexane (10 g) containing 1.01 g (7.84 mmol) of dichlorodimethylsilane in several divided portions over 15 minutes. The mixture was then gradually heated to room temperature.

WORKUP

后处理

  1. customInto a two-necked round-bottomed flask, the atmosphere in which was replaced with nitrogen
  2. customThe obtained reaction mixture in the form of a white slurry
  3. stirringwas stirred further for at 0° C. for 3 hours
  4. additionadded to a pre-cooled
  5. customover 15 minutes
  6. temperatureThe mixture was then gradually heated to room temperature