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
An amount of 20 g (0.5 mol) of sodium hydroxide and 20 ml of water were placed into a four-necked flask of 300 ml in capacity and then stirred to prepare a homogeneous solution. The temperature of this solution was reverted to room temperature, and then thereto a solution as prepared by dissolving 13.42 g (0.1 mol) of vinylbenzyl alcohol (mixture of m-isomer and p-isomer), 32.39 g (0.15 mol) of 1,4-dibromobutane, and 3.22 g (0.01 mol) of tetrabutylammonium bromide into 100 ml of toluene was added. While being vigorously stirred, the resultant mixed solution was allowed to react at 40° C. for 6 hours. Thereafter, the solution was separated and then sufficiently washed with water. The resultant organic layer was dried by adding thereto magnesium sulfate, and then toluene was distilled off under reduced pressure. The resultant solution was distilled in the presence of DPPH (diphenylpicryl-2-hydrazyl) under vacuum (boiling point: 125˜128° C./16 Pa) to obtain a colorless transparent liquid of 4-bromobutoxymethylstyrene. The yield amount was 15.0 g, and the yield ratio was 56 mol %.
WORKUP
后处理
- customto prepare a homogeneous solution
- customwas reverted to room temperature
- customa solution as prepared
- additionwas added
- stirringWhile being vigorously stirred
- additionthe resultant mixed solution
- customto react at 40° C. for 6 hours
- customThereafter, the solution was separated
- washsufficiently washed with water
- customThe resultant organic layer was dried
- additionby adding
- distillationmagnesium sulfate, and then toluene was distilled off under reduced pressure
- distillationThe resultant solution was distilled in the presence of DPPH (diphenylpicryl-2-hydrazyl) under vacuum (boiling point: 125˜128° C./16 Pa)