HRID730250

反应详情

EQUATION

反应方程式

HRID 730250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A 3 l reactor was charged under nitrogen with 11 of vinyl magnesium bromide in THF (tetrahydrofuran) and 184 g of 4-bromobutyl-dimethyl-ethoxysilane were added slowly at room temperature. The mixture was then refluxed at 70° C. for 16 h. After cooling on ice, the mixture was quenched with 407 g of a 20% HBr (w/w) solution, after which it was stirred for another 1.5 h. The THF layers were separated from the aqueous layers and neutralized with aq. sodium hydrogen carbonate solution. The THF was evaporated and the residue was distilled in the presence of 1 g Pt/C to obtain 135.8 g (79.8%) of pure 4-bromobutyl-dimethyl-vinylsilane

WORKUP

后处理

  1. additionwere added slowly at room temperature
  2. temperatureAfter cooling on ice
  3. customthe mixture was quenched with 407 g of a 20% HBr (w/w) solution
  4. customThe THF layers were separated from the aqueous layers
  5. customThe THF was evaporated
  6. distillationthe residue was distilled in the presence of 1 g Pt/C