関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Iodophenol | HCID 10784 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-cyano-4-fluoro-N-(1,2,4-thiadiazol-5-yl)benzenesulfonamide | HCID 58042302 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-cyano-4-(2-iodo-phenoxy)-N-[1,2,4]thiadiazol-5-yl-benzenesulfonamide | HCID 59436635 | 88.7% |
反応手順
To a solution of 2-iodophenol (6.0 mmol, 1320 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. for 24 hours. The reaction was cooled to room temperature and the mixture was poured into 1 N aqueous HCl (100 mL) to obtain a white solid. The afforded solid was washed with heptane and the solid was dried in vacuo to furnish 1.932 g of the title compound. LCMS Rt=1.67 minutes MS m/z 485 [MH]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541588B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-d03a31da76ca4ebf9a89d430e4f66cd3 |
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| 出典メモ | uspto-grants-2013_09 |
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