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Benzene → 9,10-Diphenylanthracene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 9,10-Dibromoanthracene | HCID 68226 | — |
| 反応物 | Phenyl dihydrogen orthoborate | HCID 78412 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 9,10-Diphenylanthracene | HCID 15159 | 75.5% |
反応手順
To a mixed solution of 286.6 g (0.85 mol) of 9,10-dibromoanthracene, 29.9 g (0.0255 mol) of Pd(PPh3)4 and 3L of benzene was added 1.5L of 2M Na2CO3aq and 1.2 L of ethanol solution of 228.6 g (1.87 mol) of phenyl boric acid, followed by refluxing for 6 hours. To the reaction solution was added 200 mL of 30% H2O2 to terminate the reaction, and an organic layer was recovered. The organic layer was washed with water and dehydrated by anhydrous magnesium sulfate, followed by filtration and concentration of the filtrate to 750 mL in total. The precipitated crystal was filtered and dried to give 212.0 g of 9,10-diphenylanthracene (Yield 75.5%, HPLC purity 97.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06566572B2 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-53d532414f0946da9b60d3647a6c3045 |
| 出典メモ | uspto-grants-2003_05 |