반응 #973856

반응 방정식

methacryloyl chloride

2-(2-(2-methyl-2-adamantyloxy)-2-oxoethoxy)-2-oxoethanol

triethylamine

p-methoxyphenol

→

2-(2-(2-methyl-2-adamantyloxy)-2-oxoethoxy)-2-oxoethyl methacrylate

수율 97.0%

용매

THF

diethyl ether

반응 조건

후처리

1. 1
   기타A 2 liter 3-neck flask fitted with a thermometer, a cooling tube and a stirrer
2. 2
   기타to form a solution
3. 3
   workup.DISSOLUTIONdissolution
4. 4
   온도the solution was cooled in an ice bath
5. 5
   기타was then returned to room temperature
6. 6
   workup.STIRRINGstirred for 3 hours
7. 7
   workup.ADDITIONwas added
8. 8
   세척the filtrate was washed 5 times with 200 ml samples of distilled water
9. 9
   추출The washed extract
10. 10
    농축was then concentrated
11. 11
    기타yielding 198 g (yield: 97%, GC purity: 99%) of the targeted colorless liquid

실험 절차

A 2 liter 3-neck flask fitted with a thermometer, a cooling tube and a stirrer was charged with 165 g (584 mmol) of 2-(2-(2-methyl-2-adamantyloxy)-2-oxoethoxy)-2-oxoethanol, 2,000 ml of THF, 105 ml (754 mmol) of triethylamine and 0.165 g (1,000 ppm) of p-methoxyphenol, and the mixture was stirred to form a solution. Following dissolution, the solution was cooled in an ice bath and 62.7 ml (648 mmol) of methacryloyl chloride was added gradually to the solution. The reaction mixture was then returned to room temperature, and stirred for 3 hours. Following completion of the reaction, 1,000 ml of diethyl ether was added, and the filtrate was washed 5 times with 200 ml samples of distilled water. The washed extract was then concentrated, yielding 198 g (yield: 97%, GC purity: 99%) of the targeted colorless liquid.

출처