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Pyridine → 1-hydroxyimino-3-phenyl-6-(3-phenylpropoxy)-1H-indene-2-carboxylic acid ethyl ester
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 | 1-oxo-3-phenyl-6-(3-phenylpropoxy)-1H-indene-2-carboxylic acid ethyl ester | HCID 11845282 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-hydroxyimino-3-phenyl-6-(3-phenylpropoxy)-1H-indene-2-carboxylic acid ethyl ester | HCID 86614026 | 58.5% |
反応手順
1-Oxo-3-phenyl-6-(3-phenyl-propoxy)-1H-indene-2-carboxylic acid ethyl ester (1.5 g, 3.64 mmol) obtained in Example 7 was dissolved in ethanol (100 mL), hydroxylamine hydrochloride (759 mg, 10.92 mmol) and pyridine (1.15 g, 15.56 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 0.91 g of the titled compound (yield: 58%).
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-ef70888cc8144573b9748559881916f2 |
| 出典メモ | uspto-grants-2010_06 |