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4-Methyl-2-nitroaniline → (4-Benzyloxy-phenyl)-(4-methyl-2-nitro-phenyl)-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methyl-2-nitroaniline | HCID 6978 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-4-phenylmethoxybenzene | HCID 138835 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | (4-Benzyloxy-phenyl)-(4-methyl-2-nitro-phenyl)-amine | HCID 66808397 | — |
反応手順
A mixture of 4-methyl-2-nitroaniline (1.006 g, 6.612 mmol), 4-benzyloxybromobenzene (5.794 g, 22.02 mmol), cuprous iodide (62.9 mg, 0.3306 mmol), potassium carbonate (0.914 g, 6.612 mmol) and anhydrous o-xylene (18 mL) was heated at 150° for 24 hours. Added additional cuprous iodide (30 mg) and heated an additional 6 hours at 160°. The reaction was cooled to room temperature and the solvent removed by rotary evaporation under vacuum. The residue was purified by silica gel flash chromatography using 1:1 methylene chloride/hexanes as eluent to afford the title compound as a red oil which slowly crystallized (1.23 g, 56%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07915411B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-5a0fae2dbaef4e53adb89bd0f05912eb |
| 出典メモ | uspto-grants-2011_03 |