참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl Anthranilate | HCID 8635 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 반응물 | 1-Bromo-9H-carbazole | HCID 11230335 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | methyl 2-(9H-carbazol-1-ylamino)benzoate | HCID 68242730 | — |
반응 단계
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%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08835626B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-a41f1b89e91147079a468a9da15166a9 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
