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Tetrahydrofuran → 5-Norbornene-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Norbornene-2-carboxylic acid | HCID 78949 | — |
反応手順
95.0 g (382 mmol) of the Diels-Alder adduct obtained in the above step was dissolved in 950 ml of tetrahydrofuran, 103 g (1.57 mol) of potassium hydroxide (85%) in 760 ml of water was added on ice cooling, and the mixture was stirred at room temperature for 24 hours. After tetrahydrofuran was distilled off from the reaction mixture, the residue was neutralized with 138 ml of concentrated hydrochloric acid, and the solution was extracted with a mixture solvent of hexane-methylene chloride (98:2) (200 ml×4). The extract was dried over anhydrous magnesium sulfate and filtered, the distilled off, and 45.0 g of crude 5-norbornene-2-carboxylic acid was obtained. Crude yield: 83%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05266728 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-b3f723c3e2834cffaf588b9c1342824e |
| 出典メモ | uspto-grants-1993_11 |