関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 4-Bromophenol | HCID 7808 | — |
| 反応物 | Methallyl alcohol | HCID 10557 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 触媒 | Sodium Tungstate Dihydrate | HCID 150191 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-(4-Bromophenoxy)-2-methylpropane-1,2-diol | HCID 71059322 | 82% |
反応手順
A mixture of β-methallyl alcohol (10 g, 139 mmol) and sodium tungstate dihydrate (92 mg, 0.28 mmol) was stirred at room temperature, and a 35% hydrogen peroxide solution (17.3 g, 153 mmol) was added thereto dropwise over a period of 5 minutes. The mixture was heated to 40° C. and stirred for 7 hours. Potassium carbonate (9.6 g, 69 mmol) and 4-bromophenol (7.9 g, 46 mmol) were added to a half amount of the resulting reaction mixture (70 mmol, based on β-methallyl alcohol), followed by stirring at 60° C. for 2.5 hours. After adding toluene (30 ml), the mixture was heated, washed with water at a temperature about 60° C., and then cooled with ice. The precipitated crystals were collected by filtration, washed with toluene (5 ml), and then dried under reduced pressure, obtaining 9.8 g of 3-(4-bromophenoxy)-2-methylpropane-1,2-diol (yield: 82% (based on 4-bromophenol)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08598358B2 |
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| 出典データセット | uspto-grants-2013_12 |
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| ORD ID | ord-4ea46972311f47e3aa328c51b872f2ca |
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| 出典メモ | uspto-grants-2013_12 |
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