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Ethanol → Ethyl 5-methylpyridine-2-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 | 5-Methylpicolinonitrile | HCID 74183 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | Ethyl 5-methylpyridine-2-carboxylate | HCID 12243769 | — |
反応手順
200 ml of ethanol and 100 ml (1.88 mol) of concentrated sulfuric acid were added to 55.5 g of 5-methylpyridine-2-carbonitrile to form a homogeneous solution, followed by heating under reflux for 2 days. The reaction liquid was gradually poured into a saturated aqueous solution of sodium hydrogencarbonate under cooling with ice to neutralize the sulfuric acid, followed by extraction with dichloromethane. The organic layer was washed with a saturated aqueous solution of common salt and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated in a reduced pressure to give 78.1 g of a brown oil of the title compound as the crude product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05789403 |
| 出典データセット | uspto-grants-1998_08 |
| ORD ID | ord-e4e75ecb96984b0594131e7871530136 |
| 出典メモ | uspto-grants-1998_08 |