HRID1982746

反应详情

EQUATION

反应方程式

HRID 1982746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customwere put into a 250 ml two-neck flask
  2. customagitation was conducted in an ice-water bath at 0° C
  3. additionslowly added to the reactants
  4. customwas conducted for an additional time of 1 hour
  5. additionThe solution was diluted
  6. custommoved to a separatory funnel
  7. washwashed with water and NaHCO3 a few times
  8. distillationdistilled under reduced pressure
  9. customto remove the solvent
  10. customPurification
  11. customto obtain a product