HRID1456913

反应详情

EQUATION

反应方程式

HRID 1456913 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

16.8 ml (0.22 moles) of a suspension of sodium in toluene at 30% are charged into a 250 ml flask. The mixture is diluted with 100 ml of THF and cooled to 0° C. 18.5 ml (0.22 moles) of cyclopentadiene diluted in 50 ml of THF are slowly added dropwise (about 60 minutes). The resulting solution is left under stirring at room temperature for a whole night, is then cooled to 0° C. and 29 ml (0.22 moles) of methoxydimethylchlorosilane fresh distillate (PETRARCH: 90%) are slowly added dropwise. The reaction is carried out at 0° C. for 3 hours. After filtration of the salt formed and evaporation of the solvent, a dark yellow oily liquid is obtained which, on distillation at 160°-162° C. gives 7.5 g of the desired product with a purity of 95.5% (GC), and a yield of 24%.

WORKUP

后处理

  1. additionare slowly added dropwise (about 60 minutes)
  2. waitThe resulting solution is left
  3. temperatureis then cooled to 0° C.
  4. filtrationAfter filtration of the salt
  5. customformed
  6. customevaporation of the solvent
  7. customa dark yellow oily liquid is obtained which
  8. distillationon distillation at 160°-162° C.