Benzophenone → Methacrylic Acid

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.

1. customwere then prepared
2. customA 5000 ml glass-jacketed reaction vessel fitted with an overhead stirrer
3. customa hose connector and septum was purged with nitrogen
4. additionAt room temperature under nitrogen, the vessel was charged with toluene (2500 ml) and 450 g of the base isobutylenelparamethylstyrene/para-bromomethylstyrene terpolymer
5. customa Mooney viscosity of 32 (1+8 min., 125° C.)
6. dissolutionThe base terpolymer was dissolved
7. stirringstirring at room temperature
8. additionThis solution was then added to the flask
9. additioncontaining the dissolved base terpolymer
10. customtemperature of 83° C
11. waitAfter 45 minutes
12. temperaturethe bath temperature was raised to 95° C.
13. waitto run for 7.5 h
14. customwas lowered to 70° C.
15. waitafter a 2.5 h period
16. temperatureto cool
17. customThe yellowish viscous solution was quenched
18. washwashed with 10 ml HCl in 1000 ml
19. washsubsequently washed with H2O/IPA (70:30) 5 to 6 times
20. customThe polymer was isolated by precipitation into 0.1% BHT in isopropanol (IPA)
21. customdried in vacuo for 48 h at 1 mm Hg and 80° C.

ORDレコード

ord-400b5388137a43afa4d6baa5d99cf25c

出典データセット

uspto-grants-1998_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05824717