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Hydrochloric Acid → 4-(Thiophen-3-yl)butanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | [2-Oxo-2-(3-thienyl)ethyl]malonic acid | HCID 6611424 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 生成物 | 4-(Thiophen-3-yl)butanoic acid | HCID 11041143 | 87.6% |
反応手順
Hydrazine hydrate (1.3 mL, 1.34 g, 26.8 mmol) was added dropwise to a solution of KOH (3.54 g, 63 mmol) and 2-[2-oxo-2-(3-thienyl) ethyl]malonic acid 8(c) (4.00 g, 17.5 mmol) in ethylene glycol (30 mL). This solution was heated at reflux for 6 hours. After cooling to room temperature, the crude reaction mixture was poured into a mixture of 6N HCl (50 mL) and ice (200 g). This aqueous mixture was saturated with NaCl, then extracted with ether (3×70 mL). The combined organic extracts were dried over Na2SO4 and concentrated, in vacuo, to provide an orange oil (2.61 g) of sufficient purity to be employed in the subsequent reaction without any further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726312 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-d7d51544825c4bb7a548bd1885f197b6 |
| 出典メモ | uspto-grants-1998_03 |