Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → N-methyl-3-nitropyridine-2-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Methylamine hydrochloride | HCID 6364545 | — |
| 반응물 | 3-Nitropyridine-2-carboxylic acid | HCID 18376612 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-methyl-3-nitropyridine-2-carboxamide | HCID 21405325 | 32% |
반응 단계
To a mixture of 3-nitropicolinic acid (8.7 g, 51.8 mmol, 1.0 eq), methylamine hydrogen chloride (4.2 g, 1.2 eq), EDC (14.9 g, 1.5 eq), HOBt (8.4 g, 1.2 eq) in DMF (30 mL) was added DIEA (54 mL, 6.0 eq). The mixture was stirred at room temperature overnight. The crude was concentrated and dissolved in EtOAc. It was washed with saturated NaHCO3 solution. The solvent was removed and the crude was purified by silica gel chromatography (20%˜80% EtOAc/Hex) to obtain the desired product N-methyl-3-nitropicolinamide (3.0 g, isolated yield 32%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08501763B2 |
| 출처 데이터셋 | uspto-grants-2013_08 |
| ORD ID | ord-bd1c65ec52a241f4a9daa8fbc4cc2667 |
| 출처 메모 | uspto-grants-2013_08 |