Methanol → 4-Vinylphenol

Temperatur

0 °C

10.0 g of p-acetoxystyrene was dissolved in 40.0 g of ethyl acetate, and the resulting solution was cooled to 0° C. Subsequently, 4.76 g of sodium methoxide (a 28 mass % methanol solution) was added dropwise over 30 minutes, and the resulting solution was stirred at room temperature for 5 hours. The organic layer was washed with distilled water three times and dried over anhydrous sodium sulfate, and the solvent was removed by distillation to obtain 13.2 g of p-hydroxystyrene (the compound represented by the following formula (1), a 54 mass % ethyl acetate solution). Thereafter, 11.0 g of a 54 mass % ethyl acetate solution of the obtained p-hydroxystyrene (1) (containing 5.9 g of p-hydroxystyrene (1)), 9.4 g of the compound represented by the following formula (2) (produced by KNC Laboratories Co., Ltd.), 2.2 g of the compound represented by the following formula (3) (produced by Daicel Corporation) and 2.3 g of polymerization initiator V-601 (produced by Wako Pure Chemical Industries, Ltd.) were dissolved in 14.2 g of propylene glycol monomethyl ether (PGME). After charging 3.6 g of PGME into a reaction vessel, the solution prepared above was added dropwise at 85° C. over 4 hours in a nitrogen gas atmosphere, and the reaction solution was heated with stirring for 2 hours and then allowed to cool to room temperature. The obtained reaction solution was added dropwise and reprecipitated in 889 g of a mixed solution of hexane/ethyl acetate (8/2 (by mass)), and the precipitate was filtered to obtain 15.5 g of (P-2).

1. washThe organic layer was washed with distilled water three times
2. dry with materialdried over anhydrous sodium sulfate
3. customthe solvent was removed by distillation

ORD-Eintrag

ord-653fc4402c4b4b14bda62e4bfe3542f4

Quelldatensatz

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09448477B2