참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methyl Methacrylate | HCID 6658 | — |
| 반응물 | 4-Methoxyphenol | HCID 9015 | — |
| 반응물 | 3-Decanol | HCID 519158 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Deca-8-yl methacrylate | HCID 22140531 | — |
반응 단계
In the same reactor as used in Example 1, 760 kg (5 kmoles) of tricyclo[5.2.1.02,6 ]deca-8-yl alcohol and 1500 kg (15 kmole) of methyl methacrylate were placed and well mixed with stirring. The water content of the resulting mixture was 2500 ppm. To the mixture, 550 g of hydroquinone monomethyl ether was added and heated while introducing thereinto dried air at a rate of 4 m3/ hr and reluxing methyl methacrylate through the distillation column to remove water by azeotropic distillation. After 1 hour from the beginning of the reflux of methyl methacrylate, the water content in the reactor became 630 ppm. Then, 3 kg of anhydrous lithium hydroxide was charged into the reactor to carry out the reaction. While removing methanol by-produced by the reaction from the reaction system by distillation, the reaction was continued until almost no methanol was distilled (about 7 hours), followed by removal of unreacted methyl methacrylate under reduced pressure. After cooling, the mixture was filtered under pressure (2 kg/cm2) using a filter paper (pore size 0.1 mm, area 5 m2) placing thereon 10 kg of diatomaceous earth to yield 990 kg of tricyclo[5.2.1.02,6 ]deca-8-yl methacrylate with the filtrating time of 2 hours.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05072027 |
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| 출처 데이터셋 | uspto-grants-1991_12 |
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| ORD ID | ord-2d7c1fd66c084b368b45f05645246858 |
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| 출처 메모 | uspto-grants-1991_12 |
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