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
After 5-norbornene-2-methanol (15 g, 0.121 mol), which was synthesized as described above, triethylamine (Aldrich, 61.2 g, 0.605 mol), and 20 ml of THF were put into a 250 ml two-neck flask, agitation was conducted in an ice-water bath at 0° C. Cinnamoyl chloride (22.1 g, 0.133 mol) was dissolved in 60 ml THF, and then slowly added to the reactants using an additional flask. After 10 min, the reactants were heated to room temperature, and agitation was conducted for an additional time of 1 hour. The solution was diluted using ethyl acetate, moved to a separatory funnel, washed with water and NaHCO3 a few times, and distilled under reduced pressure to remove the solvent. Purification was conducted using column chromatography (hexane:ethyl acetate=20:1) to obtain a product. (yield: 88%)
WORKUP
后处理
- customwere put into a 250 ml two-neck flask
- customagitation was conducted in an ice-water bath at 0° C
- additionslowly added to the reactants
- customwas conducted for an additional time of 1 hour
- additionThe solution was diluted
- custommoved to a separatory funnel
- washwashed with water and NaHCO3 a few times
- distillationdistilled under reduced pressure
- customto remove the solvent
- customPurification
- customto obtain a product