関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 2,8-Dibromodibenzofuran | HCID 82290 | — |
| 反応物 | 9-Phenyl-9H-carbazole-3-boronic acid | HCID 51358450 | — |
| 触媒 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(8-bromodibenzo[b,d]furan-2-yl)-9-phenyl-9H-carbazole | HCID 70661083 | 65% |
反応手順
A mixture of (9-phenyl-9H-carbazol-3-yl)boronic acid (1.50 g, 5.22 mmol), 2,8-dibromodibenzo[b,d]furan (2.98 g, 9.14 mmol), tetrakis(triphenylphosphine) palladium(0) (0.30 g, 0.26 mmol), potassium carbonate (2.17 g, 15.67 mmol), 1,4-dioxane (50.00 mL), and water (10.00 mL) was degassed with bubbling argon for 30 min. 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 17 (1.65 g, 65%). Confirmed by LCMS (APCI): calculated for C30H18BrNO (M+H): 488. Found: 488.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09425408B2 |
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| 出典データセット | uspto-grants-2016_08 |
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| ORD ID | ord-e2c77f4bc16c48b99a9dd32cd7a8ae87 |
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| 出典メモ | uspto-grants-2016_08 |
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