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Benzoyl Peroxide → 2,7-Dibromophenanthrene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | 2,7-Dibromo-9,10-dihydrophenanthrene | HCID 2825053 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,7-Dibromophenanthrene | HCID 11175073 | 96.4% |
反応手順
The mixture of 2,7-dibromo-9,10-dihydro-phenanthrene (2.4 g, 7.1 mmol), NBS (1.4 g, 7.8 mmol), and benzoyl peroxide (0.2 g) in carbon tetrachloride (300 ml) was refluxed for 2 hours. Potassium acetate (3.6 g) and acetic acid (3.2 ml) were added, and the refluxing was continued for additional 2 hours. The mixture was cooled and diluted with EtOAc. The organic phase was washed with water, saturated sodium bicarbonate, and brine, and was dried with sodium sulfate. Concentration gave 2,7-dibromo-phenanthrene (2.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841278B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-dabb3ebd70a24498b330d4b760d3ba56 |
| 出典メモ | uspto-grants-2014_09 |