反应 #1604334

反应方程式

3,4-di-fluoro-cinnamic acid

5-norbornene-2-methanol

xylene

→

5-norbornene 2-methyl-(3,4-di-fluoro-cinnamate)

收率 63.0%

溶剂

ethyl acetate

反应条件

后处理

1. 1
   温度azeotropically refluxed for 24 hours
2. 2
   其他After the reaction
3. 3
   温度the mixture cooled down to room temperature
4. 4
   萃取The resulting product was extracted by 1M HCl
5. 5
   洗涤washed again with water
6. 6
   干燥The organic layer was dried with Na2SO4
7. 7
   其他the solvent was evaporated out
8. 8
   其他to give a highly viscous material

实验过程

5 g (27.2 mmol) of 3,4-di-fluoro-cinnamic acid, 3.38 g (1 eq.) of 5-norbornene-2-methanol, and 0.13 g (0.02 eq.) of zirconium(IV) acetate hydroxide were added to 50 ml of xylene and stirred. The mixture was heated to 145° C. under N2 atmosphere and azeotropically refluxed for 24 hours. After the reaction, the mixture cooled down to room temperature and was added with 100 volume % of ethyl acetate. The resulting product was extracted by 1M HCl and washed again with water. The organic layer was dried with Na2SO4 and the solvent was evaporated out to give a highly viscous material. (Yield: 63%, Purity (GC): 80%)

来源