関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 9,9'-Bianthryl | HCID 66105 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 10-bromo-9,9'-Bianthracene | HCID 15195997 | 37% |
反応手順
9,9′-bianthracene (10 g, 28.2 mmol) was dissolved in DMF (200 mL), protected from light and N-bromosuccinimide (5.5 g, 31 mmol) diluted in DMF (20 ml) was added to the solution at 0° C. The reaction mixture was maintained at 0° C. for 1 hour. The solution was then warmed slowly to room temperature and stirred for 4 h. After the reaction completion, water was added to the mixture to terminate the reaction. The reaction mixture was extracted with ethyl acetate and water, dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica(hexane-dichloromethane) to give product 4.5 g (37%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09260363B2 |
|---|
| 出典データセット | uspto-grants-2016_02 |
|---|
| ORD ID | ord-bfc5c2d726484bdbb13869c20b98b247 |
|---|
| 出典メモ | uspto-grants-2016_02 |
|---|