Acetic Acid → 2-ethyl-2-adamantyl Methacrylate p-hydroxystyrene

Participants

Reaction Steps

A flask was charged with 250 g of the 2-ethyl-2-adamantyl methacrylate/p-acetoxystyrene (20:80) copolymer obtained in Reference Example 3, 10.3 g (0,084 mol) of 4-dimethylaminopyridine and 202 g of methanol, and the mixture was kept for 20 hours with stirring under reflux. After cooling, the reaction solution was neutralized with 7.6 g (0.126 mol) of glacial-acetic acid, followed by pouring into a large amount of water to obtain a precipitate. The polymer (the precipitate) thus obtained was filtered and then dissolved into acetone. An operation of pouring the solution into a large amount of water was repeated for three times to obtain a precipitate and purify the same. Amount of the obtained copolymer of 2-ethyl-2-adamantyl methacrylate and p-hydroxystyrene was 95.9 g. Also, the polymer has a weight average molecular weight of about 8,600 and a degree of dispersion of 1.65, and a copolymerization ratio thereof was determined to be about 20:80 using a nuclear magnetic resonance (13C-NMR) spectrometer. This resin will be referred to as “resin B1”.

Provenance & Evidence