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Methyl iodide → 2-(1-Methylpiperidin-3-yl)-5-(trifluoromethyl)benzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 3-(2-Nitro-4-(trifluoromethyl)phenyl)pyridine | HCID 46316762 | — |
| 触媒 | Adams' catalyst | HCID 345198 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(1-Methylpiperidin-3-yl)-5-(trifluoromethyl)benzenamine | HCID 58711919 | — |
反応手順
To an orange solution of 3-(2-nitro-4-(trifluoromethyl)phenyl)pyridine (1.4 g, 5.2 mmol) in 2 ml acetone and 1 mL benzene was added iodomethane (1.0 ml, 16 mmol). The solution was allowed to stand for 5 days, and was concentrated in vacuo to give an orange solid. A portion of this material was treated with platinum (IV) oxide (0.11 g, 0.49 mmol) in 5 ml MeOH under an atmosphere of hydrogen for approximately 24 h. The reaction was flushed with nitrogen, filtered through celite, and concentrated. Purification by silica gel chromatography (MC/MeOH/conc. NH4OH) provided the title compound. MS (m/z): 259.0 (M+H)+. Calc'd for C13H17P3N2: 258.28.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08557996B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-000fff290ab141238a506460310a9555 |
| 出典メモ | uspto-grants-2013_10 |