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Pyridine → Ethyl 3-hydroxyimino-5-methoxy-1-phenylindene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Ethyl 6-methoxy-1-oxo-3-phenyl-1H-indene-2-carboxylate | HCID 23249734 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 3-hydroxyimino-5-methoxy-1-phenylindene-2-carboxylate | HCID 73123866 | 80% |
反応手順
6-Methoxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (1.6 g, 5.19 mmol) obtained in Example 1 was dissolved in ethanol (100 mL), hydroxylamine hydrochloride (1.08 g, 15.57 mmol) and pyridine (1.64 g, 1.68 mL, 20.76 mmol) were added thereto, refluxed for 1 hr, and cooled to RT. The resulting mixture washed with saturated sodium bicarbonate and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 1.34 g of the titled compound (yield: 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745439B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-dcc48670644f41dbafba0d9dcc7475a0 |
| 出典メモ | uspto-grants-2010_06 |