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Ethanone, 1-(2,5-dichlorophenyl)- → 2-Bromo-1-(2,5-dichlorophenyl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanone, 1-(2,5-dichlorophenyl)- | HCID 75587 | — |
| 反応物 | Phenyltrimethylammonium bromide dibromide | HCID 17977687 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-1-(2,5-dichlorophenyl)ethanone | HCID 2756907 | 52.5% |
反応手順
To 2,5-dichloroacetophenone (5.0 g, 26.45 mmol) in anhydrous tetrahydrofuran (53 mL) under argon was added phenyltrimethylammonium tribromide (9.94 g, 26.45 mmol, 1.0 eq) at 0° C. The reaction mixture was stirred at ambient temperature for 16 h, concentrated, and re-dissolved in ethyl acetate. The organic layer was washed with water (2×250 mL) and brine (1×150 mL), dried (MgSO4), filtered, and evaporated in vacuo. Purification using MPLC chromatography (Biotage) gave 3.47 g (52.5%) of 2-bromo-1-(2,5-dichlorophenyl)ethanone as a clear oil. 1H-NMR (DMSO-d6) δ 7.93 (dd, J=2.1 Hz, 0.9 Hz, 1H), 7.61 to 7.60 (m, 2H), 4.86 (s, 2H);
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07384947B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-940cd5ca08984feb967880a2d7688f0b |
| 出典メモ | uspto-grants-2008_06 |