関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 4-Fluoro-4'-hydroxybenzophenone | HCID 117666 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | (4-Fluorophenyl)(4-hydroxy-3-iodophenyl)methanone | HCID 11382275 | 74% |
反応手順
(4-Fluorophenyl)(4-hydroxyphenyl)methanone (20.0 g, 92.5 mmol) in concentrated ammonium hydroxide (770 mL) was allowed to stir at 25° C. for 15 minutes and then treated with potassium iodide (74.79 g, 450.5 mmol) and iodine (23.48 g, 92.5 mmol) in water (185 mL). The reaction mixture was allowed to stir at 25° C. for 18 hours and then filtered. The precipitate was dissolved in ethyl acetate, washed with water and brine, dried, filtered and the filtrate concentrated under reduced pressure to provide the title compound as a pale green solid (23.4 g, 74% yield). 1HNMR (300 MHZ, CD3OD) δ 6.91 (d, 1H, J=8.9 Hz), 7.26 (t, 2H), 7.64 (d, 1H, J=8.9 Hz), 7.78 (t, 2H), 8.17 (s, 1H; MS (DCI) m/z 342.9 (M+H)+, 360 (M+NH4)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07538138B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-0da99411b31348cc993256a8b9a5432c |
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| 出典メモ | uspto-grants-2009_05 |
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