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Potassium Carbonate → 2-Ethyl-1-(2,4,6-triiodophenoxy)-hexane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,6-Triiodophenol | HCID 11862 | — |
| 反応物 | 2-Ethylhexyl bromide | HCID 86804 | — |
| 反応物 | 2-(2,4,6-Triiodophenoxy)butane | HCID 15814129 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Ethyl-1-(2,4,6-triiodophenoxy)-hexane | HCID 15343314 | 73.7% |
反応手順
2-Ethyl-bromohexane (10.4 g, 53.0 mmol), triiodophenol (25.5 g, 54.0 mmol) and potassium carbonate (7.5 g, 54.3 mmol) were reacted in dry DMF (110 ml) at 77° C as for 2-(2,4,6-triiodophenoxy)butane. After stirring for 20 hrs, the reaction was cooled, diluted with DMF, filtered through a pad of celite and evaporated in vacuo. The resulting residue was taken up in EtOAc (500 ml), washed with water (200 ml), 1N aqueous sodium hydroxide (200 ml), water (2×200 ml) and brine (200 ml), dried (Na2SO4), filtered and evaporated. Flash column chromatography (silica, hexanes) provided 2-ethyl-1-(2,4,6-triiodophenoxy)-hexane (22.8 g, 73.7%) as a clear viscous oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05620677 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-737e6a4871294c9197bcbc7e5927681a |
| 出典メモ | uspto-grants-1997_04 |