関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | 3-Pyridinecarboxaldehyde | HCID 10371 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,5-dimethyl-2-phenyl-3(2H)-furanone | HCID 15086699 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Phenyl-2-methyl-5-[2-(3-pyridinyl)ethenyl]-3(2H)-furanone | HCID 54185767 | 54.3% |
反応手順
To a solution of 3-pyridinecarboxaldehyde (1.03 g, 9.6 mM) and 2,5-dimethyl-2-phenyl-3(2H)-furanone (1.0 g, 8 mM) in ethanol (50 mL), was added 1N aqueous sodium hydroxide (2.4 mL, 2.4 mM). The reaction solution was heated at 60° C. for 8 hours. After the reaction solution cooled to room temperature, saturated aqueous sodium chloride (200 mL) was added. The aqueous layer was extracted with diethyl ether (3×100 mL). The combined ethereal extracts were washed with saturated aqueous sodium chloride (50 mL), dried over MgSO4, filtered and concentrated to give a brown solid. The crude product was purified by chromatography (silica gel, pet. ether-ethyl acetate) to afford a yellow crystalline solid (0.8 g, 36.3% yield), m.p. 106°-108° 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-930e8ec0b61c4a61a94ed7dd05e90d65 |
|---|
| 出典メモ | uspto-grants-1991_03 |
|---|