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Ammonium Chloride → 3-Amino-5-bromo-2-chloropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 5-Bromo-2-chloro-3-nitropyridine | HCID 7019412 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Amino-5-bromo-2-chloropyridine | HCID 21858354 | — |
反応手順
To a solution of 5-bromo-2-chloro-3-nitropyridine (5.0 g, 21.1 mmol) in methanol (50 mL) and dichloromethane (5 mL) was added zinc (7.6 g, 115.8 mmol) and ammonium chloride (5.6 g, 105.3 mmol). The reaction mixture was stirred for 24 hours. The solids were removed by filtration and washed with dichloromethane. The filtrate was washed with water (50 mL), brine (50 mL), dried over sodium sulfate, filtered and concentrated to dryness under reduced pressure. The crude 5-bromo-2-chloropyridin-3-amine (4.2 g) was used without further purification. LCMS [M+H]: 207.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541407B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-fb79ef3946d74492b5798e7221a26aa5 |
| 出典メモ | uspto-grants-2013_09 |