関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Kojic Acid | HCID 3840 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Hydroxy-2,6-bis(hydroxymethyl)-4-pyrone | HCID 2747691 | — |
反応手順
In a 100 mL round bottom flask were added Kojic acid (FLUKA, 5 g), 1N NaOH (39 mL) and H2O (10 mL). The mixture was cooled (ice/water bath) and 37% aqueous formaldehyde (ALDRICH, 2.9 mL) was added dropwise. After 34 h at room temperature additional 37% aqueous formaldehyde (ALDRICH, 0.5 mL) was added dropwise and the solution allowed to stir for 18 h. The mixture was acidified by adding concentrated HCl, and the solvent eliminated to dryness under vacuum to give a crude product which was treated with chilled water to afford a solid precipitated which was filtered and vacuum dried. 3.056 g of the title compound were obtained as a white solid. The filtrate was concentrated under vacuum and a second crop of solid separated. An additional 1.154 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07674808B2 |
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| 出典データセット | uspto-grants-2010_03 |
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| ORD ID | ord-dfd6c4d829794e1f9f992ddffcc1b375 |
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| 出典メモ | uspto-grants-2010_03 |
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