참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Potassium Acetate | HCID 517044 | — |
| 반응물 | N-(9,9-dimethylfluoren-2-yl)-2-bromoaniline | HCID 86685013 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 12,12-Dimethyl-10,12-dihydroindeno[2,1-b]carbazole | HCID 86685012 | 55.2% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09196837B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-0e6eeb2eec1d4a5dbf2cf186ce8fc35b |
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| 출처 메모 | uspto-grants-2015_11 |
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