反応 #699527
ord-dcced858d29c47d2b40b11e2319e578c
反応条件
後処理
- 1workup.STIRRINGstirring
- 2その他whereby polymerization reaction
- 3その他The resultant reaction mixture
- 4その他to precipitate a white resin
- 5その他The resin obtained
- 6その他was dried
- 7workup.DISSOLUTIONdissolved in 150 ml of methanol
- 8workup.ADDITIONThereto was added an aqueous solution
- 9その他prepared
- 10温度This mixture was heated
- 11温度with refluxing for 3 hours
- 12その他to precipitate a white resin
- 13ろ過This resin was taken out by filtration
- 14洗浄washed with water
- 15その他dried
- 16workup.DISSOLUTIONdissolved in 200 ml of tetrahydrofuran
- 17その他to give a solution, which
- 18その他reprecipitation
- 19その他The resin thus obtained
- 20その他was dried in a vacuum dryer at 120° C. for 12 hours
実験手順
In 120 ml of butyl acetate was dissolved 32.4 g (0.2 mol) of p-acetoxystyrene. Three 0.033 g portions of azobisisobutyronitrile (AIBN) were added at an interval of 2.5 hours to the solution with stirring at 80° C. in a nitrogen stream and stirring was thereafter continued for 5 hours, whereby polymerization reaction was conducted. The resultant reaction mixture was poured into 1,200 ml of hexane to precipitate a white resin. The resin obtained was dried and then dissolved in 150 ml of methanol. Thereto was added an aqueous solution prepared by dissolving 7.7 g (0.19 mol) of sodium hydroxide in 50 ml of water. This mixture was heated with refluxing for 3 hours to hydrolyze the resin. Thereafter, the reaction mixture was diluted with 200 ml of water and neutralized with hydrochloric acid to precipitate a white resin. This resin was taken out by filtration, washed with water, dried, and then dissolved in 200 ml of tetrahydrofuran to give a solution, which was added dropwise to 5 L of ultrapure water with vigorous agitation to conduct reprecipitation. This reprecipitation operation was repeated three times. The resin thus obtained was dried in a vacuum dryer at 120° C. for 12 hours to obtain poly(p-hydroxystyrene) as alkali-soluble resin A-1.