関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chlorine | HCID 24526 | — |
| 反応物 | 1-(2-Furyl)ethanol | HCID 107243 | — |
| 反応物 | Sodium Bromide | HCID 253881 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Maltol | HCID 8369 | 55% |
反応手順
In a 3-neck round bottom flask equipped with a stirring bar, a gas inlet tube and an addition funnel was added 20 ml of tetrahydrofuran, 50 ml of water and sodium bromide (0.20 mole). The solution was cooled to a temperature of 0 to 20° C. The addition funnel was charged with a solution of 1(2-furyl)-1-ethanol (0.18 mole) in 20 ml of tetrahydrofuran and this was added dropwise to the rapidly stirred reaction flask while gaseous chlorine (0.40 mole) is added via the gaseous inlet tube. The rate of the alcohol addition was such that a yellow orange color was maintained. The reaction temperature was kept below 20° C. with ice bath cooling. After the alcohol and chlorine had both been added to the reaction flask, the temperature was raised to reflux to distill off the tetrahydrofuran. The isolation procedure of Example 1 was used to isolate 12.47 g of pure maltol (55% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04368331 |
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| 出典データセット | uspto-grants-1983_01 |
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| ORD ID | ord-8b0ab203ba2540f9bc4fe8a0e4daf1f7 |
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| 出典メモ | uspto-grants-1983_01 |
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