関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methacryloyl chloride | HCID 13528 | — |
| 反応物 | 1-Ethyl-4,4-difluorocyclohexanol | HCID 66602604 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Ethyl-4,4-difluorocyclohexyl methacrylate | HCID 67969271 | 79.9% |
反応手順
A four-necked flask equipped with a stirrer, a thermometer, and a dropping funnel was charged with 6.6 g (0.04 mol) of 1-ethyl-4,4-difluorocyclohexanol, 0.2 g of 4-dimethylaminopyridine, 4.9 g of triethylamine, and 20 g of acetone. The mixture was stirred to obtain a solution. A solution prepared by dissolving 4.6 g (0.044 mol) of methacrylic acid chloride in 5 g of acetone was added to the solution at 4° C. over 30 minutes. The mixture was stirred at 4° C. for 3 hours to obtain a reaction mixture. The reaction mixture was washed with water to obtain 7.42 g of 1-ethyl-4,4-difluorocyclohexyl methacrylate (hereinafter may be referred to as “compound (M-8)” ((M-8) in Table 1)). The yield of 1-ethyl-4,4-difluorocyclohexyl methacrylate with respect to 1-ethyl-4,4-difluorocyclohexanol was 78%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08535871B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-ae4ed1cf31ce486a998b94fc968f4a3b |
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| 出典メモ | uspto-grants-2013_09 |
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