Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → Methyl 2-chloro-5-nitroisonicotinate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 2-Chloro-5-nitroisonicotinic acid | HCID 18440622 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 2-chloro-5-nitroisonicotinate | HCID 45480451 | 90.2% |
반응 단계
To a solution of 2-chloro-5-nitroisonicotinic acid (Intermediate 25A) (0.64 g, 3.17 mmol) in DMF (15 mL) under nitrogen was added sodium carbonate (1.0 g, 9.51 mmol). Reaction cooled in an ice bath and methyliodide (1.35 g, 9.51 mmol) was added dropwise. After complete addition, reaction allowed to warm to room temperature and stirred overnight under nitrogen. The reaction mixture was filtered and concentrated. The resultant crude material was purified by a 20 g silica column eluting with 40% ethylacetate in hexane to afford methyl 2-chloro-5-nitroisonicotinate (0.62 g, 2.86 mmol).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08841289B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-780c14261612436a84ead8ce4bed271c |
| 출처 메모 | uspto-grants-2014_09 |