関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | O-Methylhydroxylamine | HCID 4113 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-Methoxy-5-nitropyridine | HCID 79525 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-Amino-6-methoxy-3-nitropyridine | HCID 3852428 | 87% |
反応手順
6-Methoxy-3-nitropyridine (154 mg, 1 mmol) and O-methylhydroxylamine (71 mg, 1.5 mmol) were dissolved in DMSO (2 ml), and a resulting solution was added dropwise to a DMSO solution (3 ml) containing potassium tert-butoxide (336 mg, 3 mmol) and zinc (II) chloride (136 mg, 1 mmol) at 25° C. After completion of the addition, the resulting mixture was stirred at 25 ° C. for 9 hours and an aqueous saturated ammonium chloride solution (50 ml) was added, followed by extraction with ethyl acetate (80 ml). A resulting organic layer was dried over anhydrous magnesium sulfate, and then isolated and purified by subjection to silica gel thin layer chromatography [eluent: ethyl acetate/hexane=1/1] to obtain 147 mg of 2-amino-6-methoxy-3-nitropyridine (yield: 87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05648496 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-e2e437f90535462b87ba39f110724f13 |
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| 出典メモ | uspto-grants-1997_07 |
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