関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromodocosane | HCID 81355 | — |
| 反応物 | 2,7-Dihydroxyfluoren-9-one | HCID 4354181 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,7-Didocosyloxy-9-fluorenone | HCID 66719095 | 107.5% |
反応手順
2,7-Dihydroxy-9-fluorenone (1 g, 4.71 mmol) was dissolved in DMF (40 ml), and potassium carbonate (1.95 g, 14.1 mmol) and docosyl bromide (96%, 4.02 g, 9.91 mmol) were added. The mixture was stirred overnight at 80° C., docosyl bromide (0.40 g, 0.99 mmol) was further added and the mixture was stirred overnight. After completion of the reaction, the reaction mixture was cooled to room temperature, 1N hydrochloric acid (120 ml) was added thereto in a water bath to allow precipitation. The crystals were collected by filtration and slurry washed once with 1N hydrochloric acid (40 ml), once with pure water (40 ml) and once with methanol (40 ml) to give 2,7-didocosyloxy-9-fluorenone (4.20 g, docosyl bromide mixture).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08569453B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-a6db3e8cc7ca4091b3cfe0b06f9bf1da |
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| 出典メモ | uspto-grants-2013_10 |
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