関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Epichlorohydrin | HCID 7835 | — |
| 反応物 | 1,3-dihydroxy-12H-benzo(b)xanthen-12-one | HCID 10707705 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1,3-bis(oxiran-2-ylmethoxy)-12H-benzo[b]xanthen-12-one | HCID 46232648 | 21.8% |
反応手順
1,3-dihydroxy-12H-benzo[b]xanthen-12-one (0.15 g, 0.54 mmol) synthesized in Step 1 of Example 18, CS2CO3 (0.53 g, 1.62 mmol), and anhydrous acetone (30 mL) were charged to a dry round-bottom flask, and epichlorohydrin (0.25 g, 2.7 mmol) was added thereto with stirring using a syringe. The reaction mixture was stirred with reflux under a nitrogen atmosphere (55 to 60° C., overnight). Solid of the reaction mixture was filtered and removed, and the filtrate was concentrated under reduced pressure. The resulting residue was separated and purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:3 (v/v)) to give the title compound (15.3 mg, 21.8%) as a yellow 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-1d03c9ea32d24eaebcef6e626a5f8f1c |
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| 出典メモ | uspto-grants-2014_09 |
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