関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Hydroxy-4H-pyran-4-one | HCID 68129 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | ethyl 2-(4-oxo-4H-pyran-3-yloxy)acetate | HCID 20544471 | — |
反応手順
A mixture of 3-hydroxy-4H-pyran-4-one (1.12 g), ethyl 2-bromoacetate (1.7 g) and potassium carbonate (1.4 g) in ethanol (30 ml) was stirred at 67° to 70° C. for 75 minutes. The reaction mixture was allowed to stand at room temperature. An insoluble substance was filtereed off, and the filtrate was adjusted to pH 4 to 5 with conc. hydrochloric acid and the ethanol was removed. To the residue was added ethyl acetate, and the resultant mixture was washed with an aqueous solution saturated with sodium chloride and dried over magnesium sulfate. After removal of the solvent, the residue was chromatographed on silica gel (15 g) with an eluent (ethyl acetate:benzene= 1:5) to give crystals of ethyl 2-(4-oxo-4H-pyran-3-yloxy)acetate, mp 58° to 60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04172198 |
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| 出典データセット | uspto-grants-1979_10 |
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| ORD ID | ord-f78b6c3c67fc47a6ab5ccbc8478235ff |
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| 出典メモ | uspto-grants-1979_10 |
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