関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Epichlorohydrin | HCID 7835 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,3-Dihydroxy-xanthone | HCID 5488193 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-hydroxy-3-(oxiran-2-ylmethoxy)-9H-xanthen-9-one | HCID 10517143 | 22.4% |
反応手順
1,3-dihydroxy-9H-xanthen-9-one (1 g, 4.39 mmol) prepared in Step 1 of Example 2 and K2CO3 (1.52 g, 10.98 mmol) were added to a dry round-bottom flask, and anhydrous acetone (25 ml) was added thereto. Epichlorohydrin (1.73 mL, 21.95 mmol) was added dropwise to the reaction mixture, and the reaction liquid was stirred under reflux at a temperature of 55 to 60° C. for 6 hours. After the reaction was completed, the solvent was removed under reduced pressure. The resulting residue was separated and purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:1 (v/v)) to give the title compound (0.28 g, 22%) as a light brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846749B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-07e7999c8d4f4167b703d2f440767984 |
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| 出典メモ | uspto-grants-2014_09 |
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