関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 8-Quinolinesulfonyl chloride | HCID 29220 | — |
| 反応物 | 4-(4-Methylpiperazino)-1,2-benzenediamine | HCID 2763545 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Phenyl-8-quinolinesulfonamide | HCID 86588921 | 47.8% |
反応手順
8-Quinolinesulfonyl chloride (0.185 g, 0.81 mmol) was added to a solution of 2-amino-5-(4-methyl-1-piperazinyl)aniline (0.168 g, 0.81 mmol) and pyridine (514 mL, 6.39 mmol) in CH2Cl2. After 1 h at room temperature the mixture was washed with aq NaHCO3 (10%), dried (MgSO4) and the solvent was removed. Purification by chromatography (SiO2, CH2Cl2/MeOH/heptane, 4:1:5) gave N-2-amino-4-(4-methyl-1-piperazinyl)-]-phenyl-8-quinolinesulfonamide (0.110 g, 35%). MS (posES-FIA) m/z=found: 384.2, calcd 383.48; %); Anal. (C19H22ClN5O2S.3H2O) C, H, N, S and a small amount of the bis-sulfonylated N-{4-(4-methyl-1-piperazinyl)-2-[(8-quinolinylsulfonyl)amino]phenyl}-8-quinolinesulfonamide (0.070 g, 15%). The product: was converted to HCl salt before analysis; MS (posES-FIA) m/z=found: 589.6, calcd: 588.16; Anal. (C29H29ClN6O4S22H2O) C, H, N.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07566715B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-3d58d2ef579e403795a34ae1d0059160 |
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| 出典メモ | uspto-grants-2009_07 |
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