関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | P-Xylene | HCID 7809 | — |
| 反応物 | 4-Amino-2,6-dichloropyridine | HCID 137652 | — |
| 反応物 | N-(3-chloroquinoxalin-2-yl)-3-nitrobenzenesulfonamide | HCID 5007601 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-{3-[(2,6-dichloropyridin-4-yl)amino]quinoxalin-2-yl}-3-nitrobenzenesulfonamide | HCID 57448672 | — |
反応手順
A mixture of N-(3-chloroquinoxalin-2-yl)-3-nitrobenzenesulfonamide (1 g), 2,6-dichloropyridin-4-amine (760 mg) and p-xylene (10 mL) was heated at 135° C. with stirring overnight. Upon cooling to room temperature, the mixture was dissolved in dichloromethane, washed with 2 N HCl (2×) and brine, concentrated in vacuo to give a crude product of N-{3-[(2,6-dichloropyridin-4-yl)amino]quinoxalin-2-yl}-3-nitrobenzenesulfonamide. A small portion of this crude product was purified by HPLC to give N-{3-[(2,6-dichloropyridin-4-yl)amino]quinoxalin-2-yl}-3-nitro-benzenesulfonamide. 1H NMR (400 MHz, DMSO) δ 9.71 (s, 1H), 8.90 (s, 1H), 8.50 (d, 2H), 8.8.41 (d, 1H), 8.30 (s, 2H), 7.88-7.78 (m, 27.65 (d, 1H), 7.47-7.37 (m, 2H); MS (EI) m/z for C19H12C12N6O4S: 491.1, 493.1 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481001B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-da48f2f4c03d4794bc2192b78051f167 |
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| 出典メモ | uspto-grants-2013_07 |
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