HRID1351761

反应详情

EQUATION

反应方程式

HRID 1351761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Tricyclo[3.3.1.13,7]decanol (25 g), triethylamine (28 g) and toluene (250 g) were charged in a four-necked 500 ml flask, and then chlorodimethylvinylsilane (30 g) was dropwise added to the mixture at 40° C. over one hour while well stirring. The mixture was stirred at 40° C. for 7 hours with monitoring the progress of the reaction by gas chromatography. After the completion of the reaction, a 4% hydrochloric acid (300 ml) was added to the reaction mixture, and then the mixture was separated. The organic layer was washed with water and concentrated by evaporating off toluene contained in the organic layer, and the residue was distilled under reduced pressure to obtain 2-dimethylvinylsiloxy-tricyclo[3.3.1.13,7]decane having the following structure (40 g):

WORKUP

后处理

  1. stirringThe mixture was stirred at 40° C. for 7 hours
  2. customthe progress of the reaction by gas chromatography
  3. customAfter the completion of the reaction
  4. customthe mixture was separated
  5. washThe organic layer was washed with water
  6. concentrationconcentrated
  7. customby evaporating off toluene
  8. distillationthe residue was distilled under reduced pressure