Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Azobisisobutyronitrile → 1,1'-Biphenyl, 4'-(bromomethyl)-2-nitro-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Azobisisobutyronitrile | HCID 6547 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | 4'-Methyl-2-nitro-1,1'-biphenyl | HCID 10443194 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 생성물 | 1,1'-Biphenyl, 4'-(bromomethyl)-2-nitro- | HCID 11779072 | 37.2% |
반응 단계
A 2 L 24/40 three necked round-bottom flask equipped with a mechanical stirrer, a reflux condenser and a stopper, was charged with 15.427 g (72 mmol) of 4-methyl-2'-nitro[1,1'-biphenyl], 1.2 L of carbon tetrachloride, 14.164 g (80 mmol) of N-bromosuccinimide, and 0.50 g of 2,2'-azobis(2-methylpropionitrile). The stirred reaction mixture was refluxed under a nitrogen atmosphere for 4 hours, then cooled to room temperature and filtered. The filtrate was evaporated in vacuo and the residual oil was purified on a silica gel flash chromatography column eluted with 10% ethyl acetate-hexane. Evaporation of the pure fractions afforded the product as a yellow crystalline solid (7.83 g, 37%) which had: mp 109°-110° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05157026 |
| 출처 데이터셋 | uspto-grants-1992_10 |
| ORD ID | ord-b150302fcaab410589c6e234d12a84ae |
| 출처 메모 | uspto-grants-1992_10 |