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Tris(hydroxymethyl)aminomethane → 1-[3-(aminosulfonyl)phenyl]-8-[(2-chlorobenzoyl)amino]-1H-benzo[g]indazole-3-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| 反応物 | 2-Chlorobenzoyl chloride | HCID 69110 | — |
| 反応物 | 8-amino-1-[3-(aminosulfonyl)phenyl]-1H-benzo[g]indazole-3-carboxamide | HCID 22592523 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 1-[3-(aminosulfonyl)phenyl]-8-[(2-chlorobenzoyl)amino]-1H-benzo[g]indazole-3-carboxamide | HCID 10208180 | — |
反応手順
To a stirred solution of 8-amino-1-[3-(aminosulfonyl)phenyl]-1H-benzo[g]indazole-3-carboxamide from step 2 (76.2 mg, 0.20 mmol) in pyridine (25 mL) at RT was added 2-chlorobenzoic chloride (53 mg, 0.3 mmol). After 14 h, trisamine was added and the mixture was stirred for 2 h. The mixture was filtered through a silica gel pad with EtOAc and concentrated. The resulting title product was a solid (42 mg, 40%). Its structure was confirmed by 1H NMR and MS (521, M+1). C25H18ClN5O4S, Calc.: C: 57.75, H: 3.49; N: 13.47; Found, C: 57.06, H: 3.65, N: 13.51.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06849653B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-5f7de2e00e384a6b8a93e23288a961eb |
| 出典メモ | uspto-grants-2005_02 |