関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Methoxyphenol | HCID 9015 | — |
| 反応物 | Methacryloyl chloride | HCID 13528 | — |
| 反応物 | 2-(2-(2-Methyl-2-adamantyloxy)-2-oxoethoxy)-2-oxoethanol | HCID 58105967 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(2-(2-Methyl-2-adamantyloxy)-2-oxoethoxy)-2-oxoethyl methacrylate | HCID 57828741 | 97% |
反応手順
165 g (584 mmol) of 2-(2-(2-methyl-2-adamantyloxy)-2-oxoethoxy)-2-oxoethanol, 2,000 mL of THF, 105 mL (754 mmol) of triethylamine, and 0.165 g (1,000 ppm) of p-methoxyphenol were added to and dissolved in a 2 L three-necked flask equipped with a thermometer, a cooling pipe, and a stirrer. Following completion of the dissolution, 62.7 mL (648 mmol) of methacryloyl chloride was gradually added thereto while cooling in an ice bath. The temperature of the resultant was then elevated to room temperature, and the resultant was stirred for 3 hours. Following the completion of the reaction, 1,000 mL of diethyl ether was added thereto, followed by washing with 200 mL of distilled water 5 times. Thereafter, the extraction liquid was concentrated, thereby obtaining 198 g of an objective substance (namely, a compound 3 having the following structure) in the form of a colorless liquid (yield: 97%, GC purity: 99%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541157B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-ed19f7c11f3d4a8095282b42ad8ac6c4 |
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| 出典メモ | uspto-grants-2013_09 |
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