関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (4-Nitrophenyl)acetic acid | HCID 4661 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(4-Morpholinyl)-2-(4-nitrophenyl)ethanone | HCID 5170165 | — |
反応手順
A room temperature solution of 1.8839 gms. (4-Nitro-phenyl)-acetic acid in tetrahydrofuran (5 mL) is treated with 1.8069 gms. 1′,1′-carbonyl-diimidizole. The reaction mixture is stirred for 1 h. The reaction mixture is then treated with 1.0 mL morpholine. The reaction is heated overnight at 35° C. The reaction is then allowed to cool to room temperature, and is made basic with the addition of saturated aqueous sodium bicarbonate. The resulting mixture is extracted with ethyl acetate. The aqueous layer is re-extracted four more times with ethyl acetate. The combined organics are evaporated to dryness in vacuo. The crude product residue is then chromatographed by flash silica gel chromatography using 60% ethyl acetate in hexanes as the eluant. Following evaporation of solvent, 1-morpholin-4-yl-2-(4-nitro-phenyl)-ethanone is isolated as a white solid in the amount of 1.4009 gms.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098236B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-f62c3c18b80740c0b6b9fd0839671267 |
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| 出典メモ | uspto-grants-2006_08 |
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