参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 间溴三氟甲苯 | HCID 9817 | — |
| 反应物 | 间氨基苯甲醚 | HCID 10824 | — |
| 试剂 | 叔丁醇钠 | HCID 23676156 | — |
| 催化剂 | 4,5-双二苯基膦-9,9-二甲基氧杂蒽 | HCID 636044 | — |
| 催化剂 | 醋酸钯 | HCID 4144353 | — |
| 溶剂 | 苯甲醚 | HCID 7519 | — |
| 产物 | [3-(Trifluoromethyl)phenyl](3-methoxyphenyl)amine | HCID 82537028 | 0% |
反应步骤
PdOAc2 (8 mg, 0.04 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (40 mg, 0.07 mmol) were added to a dried vial. The vial was caped with a septa-cap and inerted with nitrogen. Degassed anisole (2 mL)was added and the catalyst mixture was heated to 50ºC for 30 minutes, then cooled down to rt. A dry 2ml microwave vial was charged with sodium 2-methylpropan-2-olate (52 mg, 0.54 mmol). It was caped and inerted with nitrogen. A degassed mixture of 1-bromo-3-(trifluoromethyl)benzene (50 µL, 0.36 mmol) and 3-methoxyaniline (50 µL, 0.45 mmol) in anisole (2 mL) wad added at rt. The catalyst solution was added to the reaction mixture. The nitrogen inlet was removed and the vial was inserted into an alumina block at 100°C. The reaction was stirred over night. After 19h, the reaction was cooled down and filtered through celite. The filtrate was concentrated. Large amounts of anisole was present. No product was detected by LCMS. The sample was descarded.
来源与证据
| 来源数据集 | 750 AstraZeneca ELN dataset |
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| ORD ID | ord-09a52aa0a68e4624905d84eed602571e |
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| 来源说明 | 750 AstraZeneca ELN dataset |
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