反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwere added dropwise
- additionDuring the addition
- temperaturethe temperature was maintained at 5° C. to 7° C
- customwas elevated to 45° C., at which
- waitwas continued for 6 hours
- customAfter the reaction
- customthe reaction was terminated with ethanol
- customthe solvent was evaporated
- additionThe residue was poured into 2 l of n-hexane
- filtrationthe insoluble are filtered off
- customfollowed by evaporation and distillation