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Dimethylamine → N,N-dimethyl-5-nitropyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N,N-dimethyl-5-nitropyridin-2-amine | HCID 75707 | 94% |
反応手順
To 0.314 g (1.99 mmol) of 2-chloro-5-nitropyridine in MeOH (1 mL) was added 5 mL of dimethylamine (2M solution in MeOH) at 0° C. and the mixture was warmed to room temperature. The reaction mixture was concentrated and extracted with EtOAc. The organic layer was washed successively with sat. NaHCO3 solution and brine, dried (Na2SO4), and concentrated to give 0.313 g (94% yield) of 2-dimethylamino-5-nitropyridine as an orange powder: 1H NMR (CDCl3) δ9.06 (d, J=2.7 Hz, 1H), 8.20 (dd, J=9.5, 2.7 Hz, 1H), 6.46 (dd, J=9.5, 0.4 Hz, 1H), 3.23 (s, 6H); LCMS (APCI+) m/z: 168 (MH+, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08486939B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-504f0d6541004dee8daa2c596cc37001 |
| 出典メモ | uspto-grants-2013_07 |