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2-Methoxyethylamine → 3-bromo-N-(2-methoxyethyl)-5-nitropyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methoxyethylamine | HCID 8018 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Bromo-2-chloro-5-nitropyridine | HCID 230889 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-bromo-N-(2-methoxyethyl)-5-nitropyridin-2-amine | HCID 79535320 | 134% |
反応手順
Triethylamine (53 μl) and 2-methoxyethylamine (23 mg) were added to a tetrahydrofuran (2 ml) solution containing 3-bromo-2-chloro-5-nitropyridine (60 mg), followed by stirring at room temperature for 1 hour. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=6:1 to 3:1), and a light yellow solid of 3-bromo-N-(2-methoxyethyl)-5-nitropyridin-2-amine (93.5 mg) was thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895585B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-6bacd450bdf6420f91e663be831853fd |
| 出典メモ | uspto-grants-2014_11 |