反应 #2069928

反应方程式

ethyl acetate

Cinnamoyl chloride

5-norbornene-2-methanol

triethylamine

→

5-norbornene 2-methylcinnamate

收率 88.0%

溶剂

THF

THF

反应条件

后处理

1. 1
   其他were put into a 250 ml two-neck flask
2. 2
   其他agitation was conducted in an ice-water bath at 0° C
3. 3
   workup.ADDITIONslowly added to the reactants
4. 4
   其他was conducted for an additional time of 1 hour
5. 5
   workup.ADDITIONThe solution was diluted
6. 6
   其他moved to a separatory funnel
7. 7
   洗涤washed with water and NaHCO3 a few times
8. 8
   workup.DISTILLATIONdistilled under reduced pressure
9. 9
   其他to remove the solvent
10. 10
    其他Purification
11. 11
    其他to obtain a product

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%)

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