Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 6-Chloro-2-methoxy-3-nitropyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,6-Dichloro-3-nitropyridine | HCID 85239 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | 6-Chloro-2-methoxy-3-nitropyridine | HCID 10797703 | — |
반응 단계
To a suspension of sodium hydride (684 mg, 28.49 mmol) in xylene (100 ml), methanol (0.98 ml, 25.9 mmol) in xylene (30 ml) was added under nitrogen. The mixture was stirred for 20 min. A solution of 2,6-dichloro-3-nitropyridine (5.0 g, 25.9 mmo) in xylene (100 ml) was added to the reaction mixture and stirred at room temperature overnight. Water (50 ml) was added and the organic layer was separated. The organics was washed with water (1×50 ml) and brine (2×50 ml), dried, and concentrated in vacuo. The crude product was purified by flash chromatography (10:1 methylene chloride and acetone) to provide the desired compound, 6-chloro-2-methoxy-3-nitro-pyridine, as the only isomer as light yellow solid (90%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425557B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-f960d4a592e84bd0a048645b99309520 |
| 출처 메모 | uspto-grants-2008_09 |