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2,4,6-Triiodophenol → 2,4,6-Triiodophenyl (2-propyl)pentanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4,6-Triiodophenol | HCID 11862 | — |
| 反応物 | 2-Propylvaleryl chloride | HCID 76240 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2,4,6-Triiodophenyl (2-propyl)pentanoate | HCID 86747892 | 68% |
反応手順
A mixture of 2,4,6-triiodophenol (2.0 g, 4.24 mmol), 2-propylvaleroyl chloride (2.5 ml, 12.7 mmol, 3 eq) and 4-dimethylaminopyridine (DMAP; 20 mg) in 20 ml of acetonitrile was refluxed under argon overnite. The reaction mixture was cooled and poured into excess aqueous sodium bicarbonate and then extracted with dichloromethane. The dichloromethane extract was dried over magnesium sulfate, filtered, and evaporated to give the crude product (2.42 mmol, 95%) as a pink solid. Recrystallization from ethyl acetate gave 1.75 g (68%) of pure product, mp 99°-101° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05468466 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-8b105aff4e6d46b4b92270d2ff404464 |
| 出典メモ | uspto-grants-1995_11 |