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9-Bromophenanthrene → HCID 86657206、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 9-Bromophenanthrene | HCID 11309 | — |
| 反応物 | 9-bromo-13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione | HCID 58175293 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 86657206 | HCID 86657206 | 64.2% |
反応手順
9-bromophenanthrene (13.88 g, 0.054 mol) was placed in a flask, and THF (200 ml) was added thereto. After dissolution, n-BuLi (38.4 ml, 0.06 mol) was gradually added at −780, and the reaction mixture was stirred for one hour at a maintained temperature. Then, 9-bromo-13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione (9.67 g, 0.024 mol) was added and the reaction mixture was stirred at room temperature for 12 hours. After the reaction was terminated, the reaction solution was washed with distilled water, extracted with ethyl acetate, and purified by column chromatography to give 9-bromo-13,13-dimethyl-6,11-di(phenanthren-9-yl)-11,13-dihydro6H-indeno[1,2-b]anthracene-6,11-diol (11.7 g, yield=64%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08525158B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-d09c11998eef444088b4328b3090a3c8 |
| 出典メモ | uspto-grants-2013_09 |