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Sodium Chloride → 2-(4-Fluorophenyl)-2-methyl-5-[2-(3-thienyl)ethenyl]-3(2H)-furanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Thiophenecarboxaldehyde | HCID 68135 | — |
| 反応物 | 2-(4-Fluorophenyl)-2,5-dimethylfuran-3(2H)-one | HCID 15086704 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(4-Fluorophenyl)-2-methyl-5-[2-(3-thienyl)ethenyl]-3(2H)-furanone | HCID 53699299 | 62% |
反応手順
To a solution of 3-thiophenecarboxaldehyde (1.3 g, 1.2 mM) and 2,5-dimethyl-2-(4-fluorophenyl)-3(2H)-furanone (2.0 g, 9.8 mM) in ethanol (75 mL), was added 1N aqueous sodium hydroxide (2 mL, 2 mM). The reaction solution was stirred at room temperature for one day. After saturated aqueous sodium chloride (400 mL) was added, the aqueous layer was extracted with dichloromethane (3×100 mL). The combined dichloromethane extracts were washed with saturated aqueous sodium chloride (50 mL), dried over MgSO4, filtered and concentrated to give a brown oil. The crude product was purified by chromatography (silica gel, pet. ether-ethyl acetate) to afford a yellow solid (1.8 g, 62% yield), m.p. 97°-98° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05001126 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-86b3919747e04f9683e021ce45808f74 |
| 出典メモ | uspto-grants-1991_03 |