関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | p-(Trifluoromethoxy)phenol | HCID 70015 | — |
| 反応物 | 2,2,6,6-Tetramethyl-3,5-heptanedione | HCID 70700 | — |
| 反応物 | N-(4-iodophenyl)methanesulfonamide | HCID 836147 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | N-[4-(4-Trifluoromethoxy-phenoxy)-phenyl]-methanesulfonamide | HCID 68514657 | — |
反応手順
To a solution of 4-trifluoromethoxy-phenol (0.7 mL, 5.4 mmol) in NMP (6 mL) was added Cs2CO3 (1.76 g, 5.4 mmol). The slurry was degassed for 2 min and added N-(4-iodo-phenyl)-methanesulfonamide (0.80 g, 2.7 mmol) from Example 33, Step A, 2,2,6,6-tetramethylheptane-3,5-dione (0.056 mL, 0.27 mmol) and CuCl (0.134 g, 1.35 mmol) subsequently. The reaction mixture was heated to 110° C. under N2 overnight. The reaction was brought to the usual work-up and the crude material was purified by chromatography (20% EtOAc/hexanes). MS (EI) 348 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07803793B2 |
|---|
| 出典データセット | uspto-grants-2010_09 |
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| ORD ID | ord-35ebee4bc113423f9af397a238b60cdc |
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| 出典メモ | uspto-grants-2010_09 |
|---|
