반응 #72404

반응 방정식

methacryloyl chloride

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

triethylamine

p-methoxyphenol

→

compound 3

수율 97.0%

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

수율 97.0%

용매

THF

diethyl ether

반응 조건

후처리

1. 1
   workup.DISSOLUTIONdissolved in a 2 L three-necked flask
2. 2
   기타equipped with a thermometer
3. 3
   workup.ADDITIONwas gradually added
4. 4
   온도while cooling in an ice bath
5. 5
   기타was then elevated to room temperature
6. 6
   workup.ADDITIONwas added
7. 7
   세척by washing with 200 mL of distilled water 5 times
8. 8
   추출Thereafter, the extraction liquid
9. 9
   농축was concentrated

실험 절차

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 were added to and dissolved in a 2 L three-necked flask equipped with a thermometer, a cooling pipe, and a stirrer. Following completion of the dissolution, 62.7 mL (648 mmol) of methacryloyl chloride was gradually added thereto while cooling in an ice bath. The temperature of the resultant was then elevated to room temperature, and the resultant was stirred for 3 hours. Following the completion of the reaction, 1,000 mL of diethyl ether was added thereto, followed by washing with 200 mL of distilled water 5 times. Thereafter, the extraction liquid was concentrated, thereby obtaining 198 g of an objective substance (namely, a compound 3 having the following structure) in the form of a colorless liquid (yield: 97%, GC purity: 99%).

출처