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Morpholine → 4-(2-Fluoro-4-nitrobenzyl)morpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 2-Fluoro-4-nitrotoluene | HCID 74025 | — |
| 触媒 | Benzoyl Peroxide | HCID 7187 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 4-(2-Fluoro-4-nitrobenzyl)morpholine | HCID 21955027 | 55% |
反応手順
2-Fluoro-4-nitrotoluene (1.55 g, 10 mmol), N-bromosuccinimide (1.82 g, 10 mmol), and benzoyl peroxide (0.1 g, 0.4 mmol) were dissolved in CCl4 (50 mL). The mixture was heated at reflux, and irradiated with light (100 W bulb) for 4 hours. The reaction mixture was then filtered and concentrated. The residue was dissolved in THF (50 mL). Morpholine (1.91 g, 22 mmol) was added to it. The mixture was stirred at ambient temperature for 1 hour and then filtered. The filtrate was evaporated. The bright orange residue was purified by column chromatography eluted with hexane:ethyl acetate, 10:1 to provide 4-(2-fluoro-4-nitrobenzyl)morpholine (1.32 g, 5.5 mmol, yield 55%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07875728B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-1f0d58fdd02945cbb88db14fdd94fc01 |
| 出典メモ | uspto-grants-2011_01 |