반응 #487061

반응 방정식

benzophenone

acrylate

methacrylate

isobutylene para-methylstyrene para-bromomethylstyrene

tetrabutylammonium hydroxide

4-hydroxybenzophenone

acrylic acid

→

acrylic acid

methacrylic acid

용매

methanol

water

반응 조건

후처리

1. 1
   기타were then prepared
2. 2
   기타A 5000 ml glass-jacketed reaction vessel fitted with an overhead stirrer
3. 3
   기타a hose connector and septum was purged with nitrogen
4. 4
   workup.ADDITIONAt room temperature under nitrogen, the vessel was charged with toluene (2500 ml) and 450 g of the base isobutylenelparamethylstyrene/para-bromomethylstyrene terpolymer
5. 5
   기타a Mooney viscosity of 32 (1+8 min., 125° C.)
6. 6
   workup.DISSOLUTIONThe base terpolymer was dissolved
7. 7
   workup.STIRRINGstirring at room temperature
8. 8
   workup.ADDITIONThis solution was then added to the flask
9. 9
   workup.ADDITIONcontaining the dissolved base terpolymer
10. 10
    기타temperature of 83° C
11. 11
    workup.WAITAfter 45 minutes
12. 12
    온도the bath temperature was raised to 95° C.
13. 13
    workup.WAITto run for 7.5 h
14. 14
    기타was lowered to 70° C.
15. 15
    workup.WAITafter a 2.5 h period
16. 16
    온도to cool
17. 17
    기타The yellowish viscous solution was quenched
18. 18
    세척washed with 10 ml HCl in 1000 ml
19. 19
    세척subsequently washed with H2O/IPA (70:30) 5 to 6 times
20. 20
    기타The polymer was isolated by precipitation into 0.1% BHT in isopropanol (IPA)
21. 21
    기타dried in vacuo for 48 h at 1 mm Hg and 80° C.

실험 절차

Terpolymer derivatives having either acrylate or methacrylate units and benzophenone moieties substituted on the isobutylene/para-methylstyrene/para-bromomethylstyrene were then prepared. A 5000 ml glass-jacketed reaction vessel fitted with an overhead stirrer, a hose connector and septum was purged with nitrogen. At room temperature under nitrogen, the vessel was charged with toluene (2500 ml) and 450 g of the base isobutylenelparamethylstyrene/para-bromomethylstyrene terpolymer above comprising 2.4 total mole percent para-methylstyrene, including 1.10 mole percent para-bromomethylstyrene, and having a Mooney viscosity of 32 (1+8 min., 125° C.). The base terpolymer was dissolved by stirring at room temperature overnight. A tetrabutylammonium salt of acrylic acid (or methacrylic acid) was prepared in a second flask by charging 101.3 ml tetrabutylammonium hydroxide (1.0M in methanol) and 7.3 ml acrylic acid (7.0 ml methacrylic acid) and 4 g of 4-hydroxybenzophenone and 30 ml of methanol to the flask and stirring at room temperature to give a water-white clear solution. This solution was then added to the flask containing the dissolved base terpolymer, at a circulating bath temperature of 83° C. After 45 minutes, the bath temperature was raised to 95° C. and let to run for 7.5 h. Then the bath temperature was lowered to 70° C., and after a 2.5 h period, the reaction was let to cool. The yellowish viscous solution was quenched and washed with 10 ml HCl in 1000 ml deionized water, and subsequently washed with H2O/IPA (70:30) 5 to 6 times. The polymer was isolated by precipitation into 0.1% BHT in isopropanol (IPA) and dried in vacuo for 48 h at 1 mm Hg and 80° C.

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