関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Anthranilate | HCID 8635 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | 1-Bromo-9H-carbazole | HCID 11230335 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | methyl 2-(9H-carbazol-1-ylamino)benzoate | HCID 68242730 | — |
反応手順
35.51 g (234.9 mmol) of methyl anthranilate are dissolved in 500 ml of toluene and degassed well. 52 g (213 mmol) of 1-bromocarbazole, 2.1 g (10.7 mmol) of 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene, 1.19 g (5.34 mmol) of Pd(OAc)2 and 76.5 g (234.9 mmol) of Cs2CO3 are added, and the mixture is then degassed and stirred at 100° C. under a protective-gas atmosphere for 24 h. The solids are subsequently filtered off via Celite, and the organic phase is washed with water, dried over MgSO4 and evaporated. The crude product is washed by stirring with hot heptane, giving 57.4 g (108 mmol), 86% of theory, purity according to HPLC 86%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09356243B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-de53838ceb6f4bbcabb63ac118599e64 |
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| 出典メモ | uspto-grants-2016_05 |
|---|
