関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Morpholinoethanol | HCID 61163 | — |
| 反応物 | 4-Fluorobenzaldehyde | HCID 68023 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(2-Morpholinoethoxy)benzaldehyde | HCID 976593 | 79.2% |
反応手順
To dried dimethylformamide (20 ml) solution in which 4-(2-hydroxyethyl)morpholine (1 g, 7.62 mmol) was dissolved, sodium hydride (201.2 mg, 8.38 mmol) was slowly added under nitrogen at room temperature. The mixture was stirred for 30 minutes at room temperature, and 4-fluorobenzaldehyde (1.1 g, 8.86 mmol) in dried dimethylformamide (5 ml) was added over 10 minutes. The reaction mixture was stirred at room temperature for 18 hours until the initial reaction product disappeared. Subsequently, 20 ml of ice water was added to the resulting mixture, and the mixture was extracted with ethyl acetate and water. The organic layer was washed with water several times, dried over anhydrous magnesium sulfate, filtered and solvent-evaporated. The residual oil was purified by silica gel column chromatography (hexane:ethyl acetate=5:1) to afford the intermediate compound 4-(2-(morpholinoethoxy)benzaldehyde (1.42 g, 79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08637558B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-f277baae6b694f46a766846b39948e35 |
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| 出典メモ | uspto-grants-2014_01 |
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