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Formic Acid → N-(2-fluoro-4-iodophenyl)formamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-Fluoro-4-iodoaniline | HCID 185694 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(2-fluoro-4-iodophenyl)formamide | HCID 23549341 | 97.1% |
反応手順
To a cooled solution (0° C.) of 4-iodo-2 fluoroaniline (3.05 g, 12.9 mmol) in tetrahydrofuran (15 mL) and toluene (15 mL), was slowly added a mixture of acetic anhydride (1.39 mL, 14.7 mmol) and formic acid (0.83 mL, 22.0 mmol). The reaction mixture was stirred at rt overnight, then diluted with ethyl acetate (100 mL) and 1N aqueous HCl (100 mL). The layers were separated, and the organic layer was washed with water and saturated sodium carbonate solution, and dried over sodium sulfate. The solvent was removed under reduced pressure to afford 2-fluoro-4-iodophenylformamide as an off-white solid (3.32 g, 97%). GC-MS ret. time 2.27 min, m/z 265 (M+); 1H NMR (300 MHz, CDCl3) δ: 7.37-7.51 (m, 3H), 8.13 (t, 1H), 8.46 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423156B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-22b4e1dc687b469fadcc66f83c4a3b41 |
| 出典メモ | uspto-grants-2008_09 |