تفاعل #72404

معادلة التفاعل

methacryloyl chloride

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

triethylamine

p-methoxyphenol

→

compound 3

المردود 97.0%

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

المردود 97.0%

المذيبات

THF

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   workup.DISSOLUTIONdissolved in a 2 L three-necked flask
2. 2
   أخرىequipped with a thermometer
3. 3
   workup.ADDITIONwas gradually added
4. 4
   درجة الحرارةwhile cooling in an ice bath
5. 5
   أخرىwas then elevated to room temperature
6. 6
   workup.ADDITIONwas added
7. 7
   غسيلby washing with 200 mL of distilled water 5 times
8. 8
   استخلاصThereafter, the extraction liquid
9. 9
   تركيزwas concentrated

الإجراء التجريبي

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%).

المصدر