反应详情

Into a 1 L-four-necked flask equipped with a stirrer, a thermometer and a distillation line, was added the obtained tri-n-octyl(2-hydroxyethyl)phosphonium chloride dissolved in 500 ml of acetonitrile. The solution was heated under a normal pressure while stirring and about 200 ml of acetonitrile was distilled. A condenser having a calcium chloride tube was installed, 1.5 g of hydroquinone monomethyl ether was added as a polymerization inhibitor, and 42.3 g (0.405 mol) of methacryloyl chloride was added thereto dropwise at 50° C. over 2 hours through a dropping funnel, then the solution was maturated for 3 hours at the same temperature as above. The absence of an unreacted substance was confirmed by FT-IR, and the reaction solution was concentrated and dried with a vacuum pump to give 209.2 g of a slightly yellow viscous liquid. The titration purity was 97.1% and the yield was 96.6%.

1. customInto a 1 L-four-necked flask equipped with a stirrer
2. temperatureThe solution was heated under a normal pressure
3. distillationabout 200 ml of acetonitrile was distilled
4. customA condenser having
5. customa calcium chloride tube was installed
6. additionwas added
7. waitthe solution was maturated for 3 hours at the same temperature
8. concentrationthe reaction solution was concentrated
9. customdried with a vacuum pump
10. customto give 209.2 g of a slightly yellow viscous liquid