참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzophenone | HCID 3102 | — |
| 반응물 | Acrylic Acid | HCID 6581 | — |
| 반응물 | 4-Hydroxybenzophenone | HCID 14347 | — |
| 반응물 | Acrylate | HCID 25188 | — |
| 반응물 | Methacrylate | HCID 87595 | — |
| 반응물 | Tetrabutylammonium Hydroxide | HCID 2723671 | — |
| 반응물 | Isobutylene p-methylstyrene p-bromomethylstyrene | HCID 69933008 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Methacrylic Acid | HCID 4093 | — |
| 생성물 | Acrylic Acid | HCID 6581 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05824717 |
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| 출처 데이터셋 | uspto-grants-1998_10 |
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| ORD ID | ord-400b5388137a43afa4d6baa5d99cf25c |
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| 출처 메모 | uspto-grants-1998_10 |
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