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Trifluoromethylsulfonamide → N-(3-{1-[5-Chloro-(4-chloro-benzyloxy)-benzyl]-5-methyl-1H-pyrazol-3-YL}-propionyl)-C,C,C-trifluoro-methanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoromethylsulfonamide | HCID 79001 | — |
| 反応物 | 3-{1-[5-Chloro-(4-chloro-benzyloxy)-benzyl]-5-methyl-1H-pyrazol-3-YL}-propionyl fluoride | HCID 86667289 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(3-{1-[5-Chloro-(4-chloro-benzyloxy)-benzyl]-5-methyl-1H-pyrazol-3-YL}-propionyl)-C,C,C-trifluoro-methanesulfonamide | HCID 86667288 | 72% |
反応手順
To a solution of acid fluoride 9 (0.14 g, 0.33 mmol) and DMAP 0.161 g (1.3 mmol) in dry DCM, trifluoromethanesulfonamide 0.147 g (0.98 mmol) was added. The mixture was stirred under a nitrogen atmosphere for 16 hours before diluting with EtOAc. The organic phase was washed with 2M HCl, followed by brine, dried over MgSO4 and evaporated to dryness. The crude acyl sulphonamide 10 was purified on silica to yield 0.13 g as a white solid (72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08492424B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-e0210d42a02c48f8befebabf8b50faf8 |
| 出典メモ | uspto-grants-2013_07 |