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Ethanol → Ethyl 1-ethyl-1H-pyrazole-5-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1-Ethyl-1H-pyrazole-5-carboxylic acid | HCID 565702 | — |
| 生成物 | Ethyl 1-ethyl-1H-pyrazole-5-carboxylate | HCID 23005846 | — |
反応手順
To a solution of 1-ethyl-1H-pyrazole-5-carboxylic acid (950 mg) (for example, available from Fluorochem) in ethanol (50 ml) was added sulphuric acid (0.5 ml) and the mixture stirred at reflux under nitrogen for 70 h. The solvent was removed in vacuo and the residue partitioned between DCM (25 ml) and saturated sodium bicarbonate solution (25 ml) and separated using a hydrophobic frit. The aqueous layer was washed with DCM (2×20 ml) and the organic phases were combined. The solvent was removed in vacuo to give the title compound (1.09 g) as a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658635B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-d52b561c3c0e42b09f4229878d584849 |
| 出典メモ | uspto-grants-2014_02 |