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Hydrochloric Acid → Dihydro-2H-pyran-4,4(3H)-dicarboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl tetrahydropyran-4,4-dicarboxylate | HCID 239606 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | Dihydro-2H-pyran-4,4(3H)-dicarboxylic acid | HCID 219303 | 92% |
反応手順
Diethyl tetrahydro-2H-pyran-4,4-dicarboxylate (4.04 g, 20 mmol) is suspended in a 30% aqueous sodium hydroxide solution (10 mL), and the mixture is stirred at room temperature for 28 hours. The pH value of the reaction solution is adjusted to pH 1 with conc. hydrochloric acid, and the mixture is separated into water and ethyl acetate. The organic layer is dried over anhydrous sodium sulfate, and the solvent is evaporated. Ethyl acetate (30 mL) is added to the obtained crude product, and the mixture is washed by repulping, and the resulting solid is collected by filtration, and dried to give tetrahydro-4H-pyran-4,4-dicarboxylic acid (3.19 g, 18.3 mmol, 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07217724B2 |
| 出典データセット | uspto-grants-2007_05 |
| ORD ID | ord-d471813f08b147ca962e4f7fd8269ef9 |
| 出典メモ | uspto-grants-2007_05 |