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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
15 g (0.121 mol) of the 5-norbornene-2-methanol prepared in Example 1, 61.2 g (0.605 mol) of triethylamine (produced from Aldrich Inc.), and 20 ml of THF were loaded into a 250 ml 2-neck flask and then stirred at 0° C. in an ice-water bath. 22.1 g (0.133 mol) of cinamoil chloride dissolved in 60 ml of THF was slowly added to the prepared mixture using an additional flask for 10 minutes. Then, the temperature of the reactant was increased to room temperature and then stirred for one hour. The resulting solution was diluted using an ethyl acetate. The diluted solution was loaded into a separatory funnel, washed using water and NaHCO3 several times, and then distilled in at a reduced pressure to remove a solvent. The result was refined using a column chromatography (Hexane:Ethyl acetate=20:1) to attain a product. (Yield: 88%)
WORKUP
后处理
- additionwas slowly added to the prepared mixture
- customfor 10 minutes
- temperatureThen, the temperature of the reactant was increased to room temperature
- stirringstirred for one hour
- additionThe resulting solution was diluted
- customThe diluted solution was loaded into a separatory funnel
- washwashed
- distillationdistilled in at a reduced pressure
- customto remove a solvent