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Water → 6-Iodohexyl-(4,4,5,5,5-pentafluoropentyl)malonic acid diethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 6-Chlorohexyl-(4,4,5,5,5-pentafluoropentyl)malonic acid diethyl ester | HCID 86760165 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 6-Iodohexyl-(4,4,5,5,5-pentafluoropentyl)malonic acid diethyl ester | HCID 86760166 | 89.4% |
反応手順
To a solution of 6-chlorohexyl-(4,4,5,5,5-pentafluoropentyl)malonic acid diethyl ester (743 mg, 1.69 mmol) in acetone (5 ml) was added sodium iodide (761 mg, 5.08 mmol), which was then refluxed for 4 h. When the reaction was completed, water was added to the reaction mixture and extracted with ethyl acetate. Then, the organic layer was washed with wafer and saturated sodium chloride solution. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (n-hexane:ethyl acetate=15:1) to give the title compound (801 mg, yield: 89%) as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07074819B2 |
| 出典データセット | uspto-grants-2006_07 |
| ORD ID | ord-7d17d3645d6548c9873294a02e062c24 |
| 出典メモ | uspto-grants-2006_07 |