関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3-Dichloroquinoxaline | HCID 16659 | — |
| 反応物 | 3-Fluorobenzenesulfonamide | HCID 150924 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(3-chloroquinoxalin-2-yl)-3-fluorobenzenesulfonamide | HCID 57625365 | 84.6% |
反応手順
3-fluorobenzenesulfonamide (250 mg, 1.4 mmol), 2,3-dichloroquinoxaline (284.1 mg, 1.4 mmol) and dry K2CO3 (198.4 mg, 1.4 mmol) are dissolved in dry DMF (0.8 ml) and heated up to 135° C. in a sealed tube for 2.5 h. When TLC confirms the completion of the reaction, the reaction mixture is cooled down to rt and quenched by addition of water (4 ml) and AcOH (0.03 ml). The residue obtained is triturated and the resulting solid is filtered and washed with water until neutral pH then dried under vacuum to afford 400 mg (83%) of the title compound as an off white solid. 1H NMR (DMSO-d6) δ 12.8-10.9 (br s, 1H), 8.05-7.62 (m, 7H), 7.54 (td, J=2.0, 8.5 Hz, 1H). HPLC (max plot) 94%; Rt 3.79 min. LC/MS: (ES+): 338.1, (ES−): 336.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08877757B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-c3076cf4b3dc4172a67b7cbff330ec16 |
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| 出典メモ | uspto-grants-2014_11 |
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