関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | N-(9,9-dimethylfluoren-2-yl)-2-bromoaniline | HCID 86685013 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 12,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole | HCID 86685012 | 55.2% |
反応手順
N-(9,9-dimethyl-9H-fluorene-2-yl)-2-bromo-aniline (18.5 g), potassium acetate (6.98 g), and DMF (95 ml) were added to a nitrogen-substituted reaction vessel and aerated with nitrogen gas for 1 hour. The mixture was heated after adding tetrakis(triphenylphosphine)palladium (1.18 g) and stirred at 100° C. for 11 hours. After the mixture was cooled to a room temperature, the reaction liquid was added to water (300 ml) and extraction was performed with toluene (300 ml). An organic layer obtained was washed with water (200 ml) twice, dehydrated with anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain a crude product. The crude product was purified by column chromatography (carrier: silica gel; eluent: toluene/n-hexane) to obtain a pale yellow powder of 12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole (7.9 g; yield 55.2%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09196837B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-0e6eeb2eec1d4a5dbf2cf186ce8fc35b |
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| 出典メモ | uspto-grants-2015_11 |
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