関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Chloride | HCID 7503 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl Maltol | HCID 21059 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Benzyloxy-2-ethyl-4-pyrone | HCID 10585542 | 65% |
反応手順
To a suspension of 2-ethyl-3-hydroxy-4-pyrone (70 g, 0.5 mol) in methanol (650 ml) and sodium hydroxide solution (24 g, 0.6 mol of sodium hydroxide dissolved in 80 ml distilled water) was added benzyl chloride (90 ml, 0.75 mol) with stirring at room temperature. The reaction mixture was refluxed for 24 hours and then cooled. The solvent was removed by rotary evaporation and the residue was extracted into dichloromethane (500 ml). The organic layer was washed with 5% w/v sodium hydroxide solution (3×600 ml) and water (2×600 ml), dried over anhydrous sodium sulphate, filtered and rotary evaporated to give an oil. This oil was crystallized from diethylether in liquid nitrogen and the product recrystallized from diethylether to give the title compound (69 g, 65%) as colourless crystals, m.p. 33°-34° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05480894 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-9f0d33d0a2f14335a2d242948edd4cec |
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| 出典メモ | uspto-grants-1996_01 |
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