反应详情

In 400 mL of isopropanol, 56.7 g of p-acetoxystyrene and 26.4 g of p-tert-butoxystyrene were dissolved, then 8.3 g of 2,2′-azobis(methyl 2-methylpropionate) (V-601: trade name of a product from Wako Pure Chemicals Ind., Ltd.) was added, followed by reacting at 80° C. for 6 hours under nitrogen gas flow. After the reaction, said reaction solution obtained was poured into 10 L of water for precipitation, followed by filtering off deposited crystal. The thus obtained crystal was added to 450 mL of methanol, followed by charging 234 g of a 15% aqueous tetramethylammonium hydroxide solution and reacting under reflux for 4 hours while stirring. The thus obtained solution was cooled to room temperature, then neutralized by adding drop-wise 12.9 g of glacial acetic acid. The neutral solution was poured into 10 L of water for precipitation, followed by filtering off deposited crystal and drying under reduced pressure, to obtain 42.6 g of poly(p-hydroxystyrene/p-tert-butoxystyrene) as a white powder crystal. The thus obtained crystal was named polymer A1. A composition ratio of p-hydroxystyrene unit and p-tert-butoxystyrene unit in polymer A1 was found to be about 7:3 from the measurement results by 13CNMR. Weight average molecular weight (Mw) of polymer A1 was about 9,500 and distribution (Mw/Mn) thereof was about 1.75 from the measurement results by gel permeation chromatography using polystyrene as a standard.

1. addition) was added
2. customAfter the reaction
3. customreaction solution
4. customobtained
5. filtrationby filtering off
6. additionThe thus obtained crystal was added to 450 mL of methanol
7. temperatureunder reflux for 4 hours
8. additionby adding drop-wise 12.9 g of glacial acetic acid
9. additionThe neutral solution was poured into 10 L of water for precipitation
10. filtrationby filtering off
11. customdrying under reduced pressure