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Azobisisobutyronitrile → 1,1'-Biphenyl, 4'-(bromomethyl)-2-nitro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 4'-Methyl-2-nitro-1,1'-biphenyl | HCID 10443194 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 1,1'-Biphenyl, 4'-(bromomethyl)-2-nitro- | HCID 11779072 | 37.2% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05157026 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-b150302fcaab410589c6e234d12a84ae |
| 出典メモ | uspto-grants-1992_10 |