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Diisopropylethylamine → 1-(3-methoxy-4-nitrophenyl)-N,N-dimethylpiperidin-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | N,N-Dimethylpiperidin-4-amine | HCID 417391 | — |
| 反応物 | 5-Fluoro-2-nitroanisole | HCID 2779250 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(3-methoxy-4-nitrophenyl)-N,N-dimethylpiperidin-4-amine | HCID 57416152 | — |
反応手順
A solution of 4-fluoro-2-methoxy-1-nitrobenzene (1.711 g, 10 mmol), N,N-dimethylpiperidin-4-amine (1.410 g, 11.00 mmol) and N-ethyl-N-isopropylpropan-2-amine (3.48 mL, 20.00 mmol) in anhydrous N,N-dimethylformamide (25 mL) was stirred at 70° C. overnight. The mixture was concentrated and the residue was mixed with water (60 mL), adjusted to pH 12, then extracted with CH2Cl2. The crude product was purified on a silica gel column eluting with 7.5% methanol in CH2Cl2 saturated with NH3 to provide the title compound. (ESI+) m/e 280.1 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536180B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-65c1901d151e45e48f0b1f53084003e2 |
| 出典メモ | uspto-grants-2013_09 |