関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Fluorene | HCID 6853 | — |
| 反応物 | Metaperiodic acid | HCID 65185 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Iodo-9H-fluorene | HCID 224094 | 644.4% |
反応手順
A 250 mL round-bottomed flask was charged with 20.0 g (120 mmol) fluorene, 16.0 g (60 mmol) iodine and 4.0 g (17 mmol) periodic acid. 150 mL (80%) acetic acid was added to the reaction mixture. The mixture was stirred under nitrogen at 80° C. for 4 hours. The mixture was then allowed to cool to ambient temperature. The solid residue was vacuum filtered, dissolved in toluene and then washed with 5% sodium hydrogen sulphite(to remove excess iodine). The toluene solution was concentrated under vacuo and then passed through a flash column using toluene as the eluent to give 32.0 g (91% yield) of the product (off white solid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07393599B2 |
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| 出典データセット | uspto-grants-2008_07 |
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| ORD ID | ord-02d49db4e29a434d840bc7c12840f8c2 |
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| 出典メモ | uspto-grants-2008_07 |
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