참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Bromo-6-methylphenol | HCID 11095329 | — |
| 반응물 | 3-cyano-4-fluoro-N-(1,2,4-thiadiazol-5-yl)benzenesulfonamide | HCID 58042302 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 59436515 | HCID 59436515 | — |
반응 단계
To a solution of 2-bromo-6-methylphenol (6.0 mmol, 1120 mg) and K2CO3 (10.5 mmol, 1450 mg) in DMF (15.0 mL) was added 3-cyano-4-fluoro-N-(1,2,4-thiadiazol-5-yl)benzenesulfonamide (Preparation 65, 4.5 mmol, 1280 mg). The reaction mixture was heated at 80° C. After stirring for overnight at 80° C., the reaction was cooled to room temperature and poured into 1 N aqueous HCl (100 mL) to precipitate which was filtered to obtain solid. The solid was washed with water (100 mL) and heptane (100 mL) and the solid was dried under vacuum to furnish the title compound. LCMS Rt=3.05 minutes MS m/z 451 [M(79Br)H]+, 453 [M(81Br)H]+ 1HNMR (d6-DMSO): δ 2.17 (s, 3H), 6.70 (d, 1H), 7.25-7.31 (m, 1H), 7.44-7.48 (m, 1H), 7.64-7.69 (m, 1H), 8.01 (dd, 1H), 8.34 (d, 1H), 8.52 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541588B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-275dae610a674b7b969fc9cc22e97dd5 |
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| 출처 메모 | uspto-grants-2013_09 |
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