関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(2-Bromophenyl)ethan-1-ol | HCID 6950331 | — |
| 反応物 | Sodium iodide dihydrate | HCID 23685997 | — |
| 触媒 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (1S)-1-(2-iodophenyl)ethanol | HCID 10514669 | 240.4% |
反応手順
To each of three identical Emrys microwave reaction vessels was added (S)-1-(2-bromophenyl)ethanol (1.67 g, 8.3 mmol), CuI (189 mg, 1.0 mmol), 1,4-dioxane (12.4 ml), N,N′-dimethylethylenediamine (0.18 ml, 1.7 mmol) and sodium iodide dihydrate (3.1 g, 16.6 mmol). Each vessel was sealed and heated in an Emrys microwave reactor to 150° C. for 2 h. On cooling, the mixtures were combined and partitioned between water (20 ml) and EtOAc (20 ml). The organic phase was washed with brine (20 ml), dried (MgSO4), filtered, and concentrated in vacuo. The crude product was taken up in isohexane (50 ml) and the solution held at −15° C. for 16 h to afford (S)-1-(2-iodophenyl)ethanol as a white crystalline solid (4.95 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07217740B2 |
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| 出典データセット | uspto-grants-2007_05 |
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| ORD ID | ord-753537b8cefe465291c457c56dfc875d |
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| 出典メモ | uspto-grants-2007_05 |
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