HRID1106130

反应详情

EQUATION

反应方程式

HRID 1106130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 300 ml four necked flask equipped with a thermometer, a reflux condenser, an inlet for nitrogen and a stirrer were charged 1860 ml of dry n-hexane and 148 g of iso-propylamine. While stirring the mixture, 119 ml of a 15% n-butyllithium n-hexane solution were added dropwise thereto. During the addition, the temperature was maintained at 5° C. to 7° C. The color of the solution was changed from colorless to pale yellow. After 10 minutes, 325 g of p-divinylbenzene having a purity of 96% were added to the mixture, whereby the color of the reaction mixture was changed to brown. Then, the inner temperature was elevated to 45° C., at which the reaction was continued for 6 hours. After the reaction, the reaction was terminated with ethanol and the solvent was evaporated. The residue was poured into 2 l of n-hexane and the insoluble are filtered off, followed by evaporation and distillation, whereby there were obtained 230 g of the product having a boiling point of 62° C.-64° C./0.08 mmHg.

WORKUP

后处理

  1. additionwere added dropwise
  2. additionDuring the addition
  3. temperaturethe temperature was maintained at 5° C. to 7° C
  4. customwas elevated to 45° C., at which
  5. waitwas continued for 6 hours
  6. customAfter the reaction
  7. customthe reaction was terminated with ethanol
  8. customthe solvent was evaporated
  9. additionThe residue was poured into 2 l of n-hexane
  10. filtrationthe insoluble are filtered off
  11. customfollowed by evaporation and distillation