化工社化工社 化学情報印刷レポート · 研究参考用
2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 2,7-Dibromophenanthrene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone | HCID 6775 | — |
| 反応物 | 2,7-Dibromo-9,10-dihydrophenanthrene | HCID 2825053 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2,7-Dibromophenanthrene | HCID 11175073 | 47.7% |
反応手順
Preparing 32.7 g of 2,7-dibromo-9,10-dihydrophenanthrene, 24.1 g of 2,3-dichloro-5,6-dicyanobenzoquinone (DDQ) and 500 milliliter of benzene as a mixture solution, the solution was refluxed with heating under an ambient atmosphere of argon gas for 64 hours. The reacted solution was cooled down to a room temperature, and further filtered. Concentrating the filtrate by means of an evaporator, the residue was washed with a use of methanol. After refining the filtered product by means of a short column, the refined product was re-crystallized with a use of toluene and as a result, 15.5 g of 2,7-dibromophenanthrene was obtained as colorless needle crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07405326B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-56df3de2a9824db3b0fe2b1e3dc6b3ed |
| 出典メモ | uspto-grants-2008_07 |