関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4,4'-Dibromobiphenyl | HCID 7110 | — |
| 反応物 | tert-Butylphosphine | HCID 123165 | — |
| 反応物 | Bis[3-(carbazol-9-yl)phenyl]amine | HCID 20648014 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | n,n,n',n'-Tetrakis[3-(carbazol-9-yl)phenyl]-4,4'-biphenyldiamine | HCID 57578467 | 164.3% |
反応手順
1.50 g of bis[3-(carbazol-9-yl)phenyl]amine, 374 mg of 4,4′-dibromobiphenyl, 370 mg of sodium tert-butoxide, 12 mg of palladium acetate[II], and 10 ml of anhydrous toluene were added in a flask under a nitrogen atmosphere. At an inner temperature of 80° C., 42 mg of tert-butylphosphine was added by using a syringe. After 6 hours of reaction at 80° C., 50 ml of toluene was added to extract the objective substance, followed by filtration. The filtrate was concentrated to dryness to obtain a crude product. The dried crude product was purified by column chromatography to obtain 880 mg (yield 61%) of Compound 3 as a white solid. The product was identified by 1H-NMR analysis (see FIG. 3). The following 56 hydrogen atoms were detected upon 1H-NMR (CDCl3) analysis. δ (ppm): 8.096-8.122 ppm (8H), 7.501-7.643 ppm (8H), 7.274-7.472 ppm (40H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08053092B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-6e22b41d671f4fbea7581f603552b35e |
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| 出典メモ | uspto-grants-2011_11 |
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