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Water → 4-(2,2,3,3,4,4,5,5-Octafluoropentyloxy)-2,3,5,6-tetrafluorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,2,3,3,4,4,5,5-Octafluoro-1-pentanol | HCID 9641 | — |
| 反応物 | Pentafluorobenzoic acid | HCID 11770 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(2,2,3,3,4,4,5,5-Octafluoropentyloxy)-2,3,5,6-tetrafluorobenzoic acid | HCID 19969101 | 46.2% |
反応手順
To a mixture of 2,3,4,5,6-pentafluorobenzoic acid (1 g) and 2,2,3,3,4,4,5,5-octafluoropentanol (1.18 g) in N,N-dimethylformamide (5 ml) was added 62% sodium hydride (0.39 g) at room temperature. The mixture was stirred at the same temperature for 1 hour, and thereto was added a mixture of water and ethyl acetate. The separated organic layer was washed with water and brine, dried over magnesium sulfate, filtered, and evaporated in vacuo. The residue was purified by chromatography on silica gel to give 4-(2,2,3,3,4,4,5,5-octafluoropentyloxy)-2,3,5,6-tetrafluorobenzoic acid (923.0 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | USH0001638 |
| 出典データセット | uspto-grants-1997_03 |
| ORD ID | ord-0017f2390d414d74bd6068e2c0f7ef96 |
| 出典メモ | uspto-grants-1997_03 |