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Sodium ethoxide → Ethyl-2-(4-pyridyl)-5-pyrimidinecarboxylic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Pyridine-4-amidine hydrochloride | HCID 2776844 | — |
| 反応物 | Ethyl 2-formyl-3-oxopropanoate | HCID 11029955 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl-2-(4-pyridyl)-5-pyrimidinecarboxylic Acid | HCID 22710304 | 15% |
反応手順
Sodium ethoxide (590 mg) was dissolved in anhydrous ethanol (50 ml) at room temperature. To the resulting solution, 4-amidinopyridine hydrochloride (1.31 g) was added, followed by the dropwise addition of a solution of ethyl 2,2-diformylacetate (1.20 g) in anhydrous ethanol (50 ml). The resulting mixture was heated under reflux for 6 hours. To the residue obtained by distilling off the solvent under reduced pressure, dichloromethane and water were added. The organic layer thus separated was dried over anhydrous sodium sulfate. After the solvent was concentrated under reduced pressure, the residue was crystallized in ethanol, whereby the title compound (279 mg, 15%) was obtained as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06747023B1 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-967aba538dbf4028b42d4705cf39787f |
| 出典メモ | uspto-grants-2004_06 |