Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Ether → HCID 178526638, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | 3-Nitrophenol | HCID 11137 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-(2-chloroethyl)-1H-imidazole hydrochloride | HCID 178478570 | — |
| 촉매 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178526638 | HCID 178526638 | — |
반응 단계
240 mg (60% in oil, 6 mmol) of sodium hydride are added slowly to a solution of 1.67 g (12 mmol) of 3-nitrophenol in 10 ml of dimethylformamide and the mixture is stirred at room temperature for 1 hour. 200 mg (1.2 mmol) of 4-(2-chloroethyl)-1H-imidazole hydrochloride and tetrabutylammonium iodide (catalyst) are added and the mixture is stirred at 80° C. for 3 days. The reaction mixture is cooled and 150 ml of diethyl ether are added. The precipitate is separated by filtration and the filtrate is evaporated under reduced pressure to give a residue which is purified by preparative high performance chromatography. The title compound is converted to the oxalate and crystallized from ethanol, M.p.: 174°-178° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05708171 |
| 출처 데이터셋 | uspto-grants-1998_01 |
| ORD ID | ord-b3b65b39165a4864ac2952cb09063ec7 |
| 출처 메모 | uspto-grants-1998_01 |