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Ethanol → 5-Bromo-N-methyl-3-nitropyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 5-Bromo-2-chloro-3-nitropyridine | HCID 7019412 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Bromo-N-methyl-3-nitropyridin-2-amine | HCID 10868149 | — |
反応手順
To a solution of 5-bromo-2-chloro-3-nitropyridine (Matrix, Columbia, USA, 9.8 g, 41.3 mmol) in 250 ml THF was added 8 M methylamine in EtOH (Aldrich, Buchs, Switzerland, 12.9 ml, 103 mmol). The reaction mixture was stirred 1 h at rt then was quenched with 300 ml water. The precipite was filtered and the filtrate concentrated before being filtered again. The yellow solids were combined and dried to give the title compound as a yellow solid (HPLC: tR 3.13 min (Method A)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08476294B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-a355d5361bce4509af81f3ec9290f393 |
| 出典メモ | uspto-grants-2013_07 |