関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Benzamide, N-(4-aminophenyl)- | HCID 87196 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 反応物 | 4-Chloro-6,7,8,9-tetrahydro-5H-dipyrido[2,3-b;3',4'-d]pyrrole | HCID 66677972 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | N-[4-(6,7,8,9-Tetrahydro-5H-dipyrido[2,3-b;3',4'-d]pyrrol-4-ylamino)-phenyl]-benzamide | HCID 46843080 | 37.4% |
反応手順
4-Chloro-6,7,8,9-tetrahydro-5H-dipyrido[2,3-b;3′,4′-d]pyrrole (500 mg, 1.78 mmol), N-(4-Amino-phenyl)-benzamide (454 mg, 2.14 mmol), Pd(OAc)2 (20 mg, 0.09 mmol), X-Phos (85 mg, 0.18 mmol), and KOH (300 mg, 5.35 mmol) were dissolved in tert-butanol (9.0 mL), and stirred overnight at 100° C. The reaction mixture was concentrated, and then suspended in EtOAc/H2O. The resulting precipitate was filtered, washed with EtOAc/H2O, and dried under vacuum to provide 1 (255 mg, 37% yield) as a tan solid. LC-MS (M+H=384, obsd.=384).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08853391B2 |
|---|
| 出典データセット | uspto-grants-2014_10 |
|---|
| ORD ID | ord-3499e09f59414261905778bb3ef10ebb |
|---|
| 出典メモ | uspto-grants-2014_10 |
|---|
