4-Methoxyphenol → HCID 18779287、化合物

反応式

[Cl-].[CH2:2]([P+:6]([CH2:15][CH2:16][CH2:17][CH3:18])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:7][CH2:8][CH2:9][OH:10])[CH2:3][CH2:4][CH3:5].COC1C=CC(O)=CC=1.[C:28]([Cl:33])(=[O:32])[C:29]([CH3:31])=[CH2:30]>C(#N)C>[Cl-:33].[CH2:11]([P+:6]([CH2:2][CH2:3][CH2:4][CH3:5])([CH2:15][CH2:16][CH2:17][CH3:18])[CH2:7][CH2:8][CH2:9][O:10][C:28](=[O:32])[C:29]([CH3:31])=[CH2:30])[CH2:12][CH2:13][CH3:14]

参加物

実験手順

Into a 1 L-four-necked flask equipped with a stirrer, a thermometer and a distillation line, was added the obtained tri-n-butyl(3-hydroxypropyl)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 75.8 g (0.725 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 using FT-IR, and the reaction solution was concentrated and dried with a vacuum pump to give 290.3 g of a slightly yellow liquid. The titration purity was 94.6% and the yield was 100.0%.