참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,3-Dichloroquinoxaline | HCID 16659 | — |
| 반응물 | 3-Fluorobenzenesulfonamide | HCID 150924 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-(3-chloroquinoxalin-2-yl)-3-fluorobenzenesulfonamide | HCID 57625365 | 84.6% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08877757B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-c3076cf4b3dc4172a67b7cbff330ec16 |
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| 출처 메모 | uspto-grants-2014_11 |
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