반응 #2021471

반응 방정식

ethyl lithium

2-adamantanone

methacryloyl chloride

→

2-ethyl-2-adamantyl methacrylate

수율 60.0%

용매

diethyl ether

diethyl ether

반응 조건

후처리

1. 1
   기타A solution was prepared
2. 2
   기타under 10° C.
3. 3
   workup.ADDITIONwas added dropwise
4. 4
   기타under 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
   기타Then precipitated inorganic salts
8. 8
   기타were removed by filtration
9. 9
   세척The organic layer was washed with 5% aqueous sodium hydrogen carbonate solution
10. 10
    세척washed twice with water
11. 11
    농축The organic layer was concentrated
12. 12
    workup.DISTILLATIONdistilled under reduced pressure

실험 절차

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:

출처