反应 #2021471

反应方程式

ethyl lithium

2-adamantanone

methacryloyl chloride

→

2-ethyl-2-adamantyl methacrylate

收率 60.0%

溶剂

diethyl ether

diethyl ether

反应条件

后处理

1. 1
   其他A solution was prepared
2. 2
   其他under 10° C.
3. 3
   workup.ADDITIONwas added dropwise
4. 4
   其他under 10° C.
5. 5
   workup.ADDITIONAfter the completion of addition
6. 6
   workup.STIRRINGthe solution was stirred at room temperature for 12 hours
7. 7
   其他Then precipitated inorganic salts
8. 8
   其他were removed by filtration
9. 9
   洗涤The organic layer was washed with 5% aqueous sodium hydrogen carbonate solution
10. 10
    洗涤washed twice with water
11. 11
    浓缩The organic layer was concentrated
12. 12
    workup.DISTILLATIONdistilled under reduced pressure

实验过程

A solution was prepared by adding 50 parts of diethyl ether to 31.1 parts of 2-adamantanone. While keeping the temperature of the solution at or under 10° C., 200 ml of a diethyl ether solution containing ethyl lithium at a concentration of 1.14 mole/liter was added dropwise thereto. The solution was stirred at 0° C. for 2 hours, and then, while keeping the temperature of the solution at or under 10° C., 26.2 parts of methacryloyl chloride (1.2 mole based on 2-methyl-2-adamantanol) was added dropwise. After the completion of addition, the solution was stirred at room temperature for 12 hours. Then precipitated inorganic salts were removed by filtration. The organic layer was washed with 5% aqueous sodium hydrogen carbonate solution and then washed twice with water. The organic layer was concentrated and distilled under reduced pressure to give 2-ethyl-2-adamantyl methacrylate represented by the following formula in 60% yield:

来源