Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 1-Methyl-4-nitroimidazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | HCID 178526856 | HCID 178526856 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1-Methyl-4-nitroimidazole | HCID 18209 | 82% |
반응 단계
To a mixture of 4-nitro-1H-imidazole (2.0 g, 17.7 mmol) and K2CO3 (3.67 g, 26.5 mmol) in acetonitrile (20 mL) was added iodomethane (1.3 mL, 3.0 g, 21.2 mmol) dropwise while stirring at room temperature. The resulting mixture was stirred at 60° C. overnight. It was then evaporated under reduced pressure and the residue was diluted with water (20 mL). The mixture was extracted with dichloromethane (2×20 mL). The combined extract was concentrated under reduced pressure and the residue was purified by silica-gel column chromatography eluting with 100:1 dichloromethane/methanol to afford 268a as a yellow solid (1.8 g, 82%). MS-ESI: [M+H]+ 128.1. 1H NMR (500 MHz, DMSO-d6) δ 8.37 (s, 1H), 7.82 (s, 1H), 3.76 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09238655B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-ccce70faddf24b1aa6c2236363b886a1 |
| 출처 메모 | uspto-grants-2016_01 |