Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
O-Methylhydroxylamine → 3-Amino-4-nitropyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | O-Methylhydroxylamine | HCID 4113 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 4-Nitropyridine | HCID 70734 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl acetate hexane | HCID 21226206 | — |
| 생성물 | 3-Amino-4-nitropyridine | HCID 586943 | 25.2% |
반응 단계
4-Nitropyridine (124 mg, 1 mmol) and O-methylhydroxylamine (71 mg, 1.5 mmol) were dissolved in DMF (2 ml), and a resulting solution was added dropwise to a DMF 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 at 25° C. for one hour 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 subjecting to silica gel thin layer chromatography (eluent: ethyl acetate/hexane=1/1] to obtain 35 mg of 3-amino-4-nitropyridine (yield: 25%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05648496 |
| 출처 데이터셋 | uspto-grants-1997_07 |
| ORD ID | ord-f352db06847e43c7b3aa6d376b97850d |
| 출처 메모 | uspto-grants-1997_07 |