関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chloroaniline | HCID 7240 | — |
| 反応物 | Benzene, 2-bromo-1,4-dimethoxy- | HCID 91353 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,4-Dimethoxy-9H-carbazole | HCID 14529304 | 55% |
反応手順
Following a published procedure (Bedford, R. B.; Betham, M. J. Org. Chem. 2006, 71, 9403-9410), NaOtBu (0.754 g, 7.84 mmol), Pd(OAc)2 (0.014 g, 0.06 mmol), and [HPtBu3][BF4](0.023 g, 0.078 mmol) were suspended in dry toluene (5 mL) in a microwave vial. 2-Chloroaniline (0.165 mL, 1.567 mmol) and 2-bromo-1,4-dimethoxybenzene (0.240 mL, 1.598 mmol) were then added, and the vial was sealed. The reaction was then heated in the microwave reactor at 170° C. for 4 h, allowed to cool, and then quenched by addition of 1M HCl. The aqueous phase was extracted with CH2Cl2, the organic layer was dried over Na2SO4, filtered and condensed. The crude mixture was purified by chromatography (SiO2, 0-10% EtOAc/Hexane) to afford the title product (0.193 g, 55%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08735440B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-ed49843d2a5941e781b601c1a230fb14 |
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| 出典メモ | uspto-grants-2014_05 |
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