関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Hexen-1-ol | HCID 69963 | — |
| 反応物 | 2-Bromo-2-methylpropionyl bromide | HCID 88685 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Hex-5-EN-1-YL 2-bromo-2-methylpropanoate | HCID 20829612 | 70% |
反応手順
5-Hexen-1-ol (42.6 g), triethylamine (45.8 g), and tetrahydrofuran (0.8 L) were mixed. After ice cooling, 2-bromoisobutyryl bromide (100 g) was dropped. The reaction liquid was stirred at 4° C. for 3 hours, and then at room temperature for 15 hours. The reaction liquid was then filtered, concentrated with an evaporator, and dissolved in diethyl ether (300 mL). The solution was washed with a 1N hydrochloric acid solution (2×300 mL), a saturated sodium bicarbonate solution (2×300 mL), and distilled water (2×300 mL), in this order. After that, the organic layer was dried over sodium sulfate, filtered, and concentrated with an evaporator. The product was then purified through a silica gel column (developing solvent: hexane/ethyl acetate=15/1), and concentrated to give 74.2 g of 5-hexenyl 2-bromo-2-methylpropanate of the following chemical formula (compound 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434794B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-b22f08d90f174701a059f2bb7641776a |
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| 出典メモ | uspto-grants-2016_09 |
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