化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 3-cyano-4-fluoro-N-(1,2,4-thiadiazol-5-yl)benzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 5-Amino-1,2,4-thiadiazole | HCID 290274 | — |
| 反応物 | 3-Cyano-4-fluorobenzenesulfonyl chloride | HCID 2778908 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-cyano-4-fluoro-N-(1,2,4-thiadiazol-5-yl)benzenesulfonamide | HCID 58042302 | — |
反応手順
Sodium hydroxide (5.08 g, 0.127 mol) was dissolved in water (60 mL) and 1,4-1,4-dioxane (300 mL). 1,2,4-Thiadiazol-5-amine (10 g, 0.1 mol) was added and the reaction stirred for 5 minutes. 3-Cyano-4-fluorobenzene-1-sulfonyl chloride (8.25 g, 0.0376 mol) was added and the reaction was allowed to stir for 3 hours at 20° C. After this time, the reaction was poured into 150 mL of 1N HCl. This solution was extracted with ethyl acetate (3×50 mL). The combined organics were dried over sodium sulfate, filtered and concentrated to give the title compound as a brown solid. LCMS Rt=1.22 minutes MS m/z 283 [MH]+1H NMR (d6-DMSO) δ 8.54 (s, 1H), 8.39 (dd, 1H), 8.19 (m, 1H), 7.71 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541588B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-68e8e1545797488bab85a027743f56dc |
| 出典メモ | uspto-grants-2013_09 |