참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Butylamine | HCID 8007 | — |
| 반응물 | Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1) | HCID 62802 | — |
| 반응물 | Tinuvin 770 | HCID 164282 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Methyl Methacrylate/Butyl Acrylate Methyl Methacrylate | HCID 19810764 | — |
반응 단계
The methyl methacrylate-n-butyl acrylate diblock copolymer (150 g) was dissolved into 240 mL of toluene and placed into a 1 L reactor equipped with an agitator, a thermometer, a nitrogen gas inlet tube, a dropping funnel, and a reflux condenser. In a nitrogen atmosphere, 15 g of n-butylamine as a primary amine compound and 9 g of bis(2,2,6,6,-tetramethyl-4-piperidyl)sebacate as a HALS were added into the reactor, and stirring was performed at 50° C. for 5 hours. 1H NMR measurement and IR measurement confirmed that the thiocarbonylthio groups were converted into mercapto groups at a yield of 91%. The toluene solution of the polymer was poured into 1 L of methanol to precipitate the polymer, followed by filtration, washing with methanol, and drying. Next, the polymer was dissolved into 240 mL of toluene, and 264 mg of dichloride succinate as a polyvalent acyl halide used in method (vii) was added thereinto, followed by stirring at 60° C. for 6 hours. 1H NMR and GPC measurement confirmed that the mercapto groups were coupled at a yield of 94% by acylation. In the resultant methyl methacrylate-n-butyl acrylate-methyl methacrylate triblock copolymer, Mn=85,200 and Mw/Mn=1.66. The weight ratio of the individual constituents was the same as that before the coupling reaction.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07211625B2 |
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| 출처 데이터셋 | uspto-grants-2007_05 |
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| ORD ID | ord-2180aa3e490a430eb5fe6d958d7b0f9a |
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| 출처 메모 | uspto-grants-2007_05 |
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