反应 #1801142

反应方程式

ethyl acetate

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
   workup.ADDITIONwas slowly added to the prepared mixture
2. 2
   其他for 10 minutes
3. 3
   温度Then, the temperature of the reactant was increased to room temperature
4. 4
   workup.STIRRINGstirred for one hour
5. 5
   workup.ADDITIONThe resulting solution was diluted
6. 6
   其他The diluted solution was loaded into a separatory funnel
7. 7
   洗涤washed
8. 8
   workup.DISTILLATIONdistilled in at a reduced pressure
9. 9
   其他to remove a solvent

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%)

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