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Hydrochloric Acid → 2-Chloro-4-methoxypyridin-3-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 3-Amino-4-methoxypyridine | HCID 5200343 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 2-Chloro-4-methoxypyridin-3-amine | HCID 15790053 | 80% |
反応手順
To a magnetically stirred mixture of 3-Amino-4-methoxypyridine (4.45 g, 35.89 mmole) in 12N HCl (25 mL) cooled in an ice bath was added hydrogen peroxide (5.3 g, 46.65 mmol, 30% solution). The reaction was allowed to slowly warm to room temperature and stirred for 1 h. TLC (50% ethyl acetate/hexane) indicated complete consumption of starting material. The reaction mixture was slowly poured into saturated sodium bicarbonate solution (400 mL) to neutralize the reaction and extracted with ethyl acetate. The resulting organic layers were washed with saturated sodium chloride solution and dried over magnesium sulfate. Filtration and concentration gave 3-Amino-2-chloro-4 methoxypyridine (4.56 g, 28.77 mmol, 80% yield) as an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07947692B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-2548548e228445b1832b59a62bec1785 |
| 出典メモ | uspto-grants-2011_05 |