참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 2,8-Dibromodibenzofuran | HCID 82290 | — |
| 반응물 | 9-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-9H-carbazole | HCID 11850073 | — |
| 촉매 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 9-(4-(8-bromodibenzo[b,d]furan-2-yl)phenyl)-9H-carbazole | HCID 117607253 | 70.5% |
반응 단계
A mixture of Compound 11 (2.00 g, 4.56 mmol), 2,8-dibromodibenzo[b,d]furan (2.60 g, 7.98 mmol), tetrakis(triphenylphosphine) palladium(0) (0.26 g, 0.23 mmol), potassium carbonate (1.892 g, 13.70 mmol), 1,4-dioxane (60.00 mL), and water (12.00 mL) was degassed with bubbling argon for 1 hour. The reaction mixture was then heated to 80° C. and was stirred overnight (16.5 hours), maintaining an argon atmosphere. Consumption of the starting material was confirmed by thin-layer chromatography and the reaction was cooled to room temperature. The product was extracted with dichloromethane, dried, and purified by silica gel column chromatography with dichloromethane in hexanes as the eluent. The product fractions were then dried and the product was collected to yield Compound 13 (1.57 g, 70%). Confirmed by LCMS (APCI): calculated for C30H18BrNO (M+H): 488. Found: 488.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09425408B2 |
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| 출처 데이터셋 | uspto-grants-2016_08 |
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| ORD ID | ord-4a6647a0dcde4912a868e38fb57a2e91 |
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| 출처 메모 | uspto-grants-2016_08 |
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