반응 #1463491

반응 방정식

pyridine

1,4-dioxane

2-methoxypropene

4-toluenesulfonic acid

→

4-(1-methoxy-1-methylethoxy)styrene 4-(1-methoxy-1-methylethoxy)vinylcyclohexane 4-hydroxystyrene 4-vinylcyclohexanol

반응 조건

후처리

1. 1
   세척the reaction solution is subsequently eluted slowly through a column into which 50.0 g of a strongly basic macroporous anion exchanger
2. 2
   세척have been washed
3. 3
   기타The polymer is precipitated
4. 4
   workup.ADDITIONby introducing the reaction solution
5. 5
   workup.ADDITIONinto a mixture of water and isopropanol
6. 6
   여과filtered off with suction
7. 7
   세척washed with a mixture of water and isopropanol
8. 8
   기타dried to constant weight

실험 절차

24.0 g of 2-methoxypropene are slowly added dropwise at 10° C. to a solution of 20.0 g of partially hydrogenated poly-4-hydroxystyrene (Maruka Lyncur PHM-C, content of cycloaliphatic structural units about 10 mol %), a catalytic quantity of 4-toluenesulfonic acid and a catalytic quantity of pyridine in 140 ml of 1,4-dioxane. The reaction mixture is stirred at room temperature for 24 h; the reaction solution is subsequently eluted slowly through a column into which 50.0 g of a strongly basic macroporous anion exchanger based on sytrene/divinylbenzene copolymer (Amberlyst® A-26) have been washed. The polymer is precipitated by introducing the reaction solution into a mixture of water and isopropanol, filtered off with suction, washed with a mixture of water and isopropanol and dried to constant weight. 24.0 g of poly[4-(1-methoxy-1-methylethoxy)styrene/4-(1-methoxy-1-methylethoxy)vinylcyclohexane/4-hydroxystyrene/4-vinylcyclohexanol] are obtained, in which according to thermogravimetric analysis (TGA) 65 mol % of the original OH groups have been protected.

출처