関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dodecylbenzene | HCID 31237 | — |
| 反応物 | 3,5-Bis(1,1-dimethylethyl)-2-hydroxybenzoic acid | HCID 88208 | — |
| 反応物 | 2-Bromo-9,9-dimethylfluorene | HCID 10945606 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 反応物 | 12,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole | HCID 86685012 | — |
| 触媒 | Copper | HCID 23978 | — |
| 生成物 | HCID 86685020 | HCID 86685020 | 80.2% |
反応手順
12,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole synthesized in Example 1 (5.5 g), 2-bromo-9,9-dimethyl-9H-fluorene (6.4 g), sodium bisulfite (0.3 g), a copper powder (0.1 g), 3,5-di(tert-butyl)salicylic acid (0.5 g), potassium carbonate (4.0 g), and dodecylbenzene (5 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 180° C. for 29 hours. The mixture was cooled to 100° C., and insoluble matter was removed by filtration after adding toluene (80 ml), and a filtrate was concentrated. Crystallization using n-hexane (20 ml) was performed to obtain an ocher powder of 12,12-dimethyl-10-(9,9-dimethyl-9H-fluorene-2-yl)-10,12-dihydroindeno[2,1-b]carbazole (7.4 g; yield 80.0%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09196837B2 |
|---|
| 出典データセット | uspto-grants-2015_11 |
|---|
| ORD ID | ord-dd83ce3cc8cf4d9e9e690d815fd0a03a |
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| 出典メモ | uspto-grants-2015_11 |
|---|
